Ion chromatography system for exchanging an ion exchanger in a suppressor and a suppressor means

SOLID PHASE EXTRACTION PIPETTE

Solid phase extraction devices for sample preparation are disclosed, comprising a hollow conical tube having one narrower opening and one broader opening, wherein the narrower opening of the tube contains a solid phase extraction material comprising a functionalized monolithic sorbent, and wherein the solid phase extraction device is prepared by a combination of reduced pressure, positive pressure and mechanical compaction. The solid phase extraction devices are adapted for preparation of small sample volumes, and provide excellent recovery of analytes and good flow characteristics. Methods for preparing and using the solid phase extraction devices are disclosed.

RIGID SILICA CAPILLARY COLUMN FOR USE IN CHROMATOGRAPHY

A tubular assembly especially adaptable to capillary columns for use in gas chromatography, comprises a silica capillary wound on and fused to a silica mandrel and stress relieved by heating. The entire assembly is rigid and is more resistant to fractures than prior available columns. Variants include rigid assemblies integral with heating means. Solid, brittle stationary phases can be readily accommodated in these assemblies because of their rigidity and structural strength.

DEACTIVATED CAPILLARY COLUMNS FOR USE IN CAPILLARY ELECTROPHORESIS

PATENT APPLICATION of COLE L. WOOLLEY for DEACTIVATED CAPILLARY COLUMNS FOR USE IN CAPILLARY ELECTROPHORESIS Docket 90-107 JET/iav The wails of fused-silica capillary columns used for capillary zone electrophoresis and micellar electrokinetic capillary chromatography may be deactivated with polysiloxanes, polysilazanes and other silicone polymers to permit more effective separations without eliminating electro-osmotic flow within the columns. i ...

MULTI COLUMN CHROMATOGRAPHY SYSTEM

The present invention relates to a method and apparatus for chromatographically analyzing each of a plurality of samples in detector, comprising an autosampler to contain a plurality of samples for chromatographic analysis and a plurality of chromatographic systems, each system comprising one or more pumps and one or more chromatography columns. A detector is included for detecting compounds in the samples from each of the chromatography systems along with a valve positioned between the detector and the plurality of chromatography systems, the valve permitting each sample to reach the detector in sequence. A computer control device is included which adjusts the introduction of samples from the autosampler into the plurality of chromatography systems as well as the position of the valve to sequentially separate and deliver compounds within the samples to the detector.

High efficiency sol-gel gas chromatography column

A capillary column (10) includes a tube structure having inner walls (14) and a sol-gel substrate (16) coated on a portion of inner walls (14) to form a stationary phase coating (18) on inner walls (14). The sol solution used to prepare the sol-gel substrate (16) has at least one baseline stabilizing reagent and at least one surface deactivation reagent resulting in the sol-gel substrate (16) having at least one baseling stabilizing reagent residual and at least one surface deactivating reagent residual. A method of making the sol-gel solution is by mixing suitable sol-gel prescursors to form the solution, stabilizing the solution by adding at least one baseline stabilization reagent, deactivating the solution by adding at least one surface deactivation reagent to the solution, and reacting the solution in the presence of at least one catalyst.

Multicapillary column for chromatography and sample preparation

A multicapillary column especially useful for liquid chromatography and sample preparation comprising a plurality of uniform capillaries coated with an insoluble stationary phase, wherein the thickness of the stationary phase is correlated with the radius of the individual capillaries for high efficiency.

Open Tubular Capillaries Having a Connecting Layer

The invention relates to a method for producing open tubular capillaries containing monolithic sorbents and to said capillaries. The inventive capillaries are characterised by a connection layer between the capillary wall and the sorbent, said layer ensuring a particularly good adhesion of the sorbent to the capillary wall.

Suppression of electroosmosis with hydrolytically stable coatings

Surfaces of silica-containing materials, such as the inner walls of silica capillaries, used in chromatographic, particularly electrophoretic, separations are coated with an organic polymer layer to reduce or eliminate surface charges. The layer is applied by first converting the silanol groups on the surface to silicon halide groups, then reacting these groups with an organometallic reagent having a terminal ethenyl moiety, preferably vinyl or allyl lithium or a vinyl or allyl magnesium halide, to convert the silicon halide groups to Si--R groups where the R retains the terminal ethenyl moiety, and finally reacting these ethenyl groups newly attached to the surface with a neutral organic monomer in an addition polymerization reaction to form a monomolecular noncrosslinked polymer layer over the surface. The resulting polymer layer is linked to the silica directly through a Si--C bond which is stable over a wide range of pH conditions.

GAS CHROMATOGRAPH COLUMN WITH CARBON NANOTUBE-BEARING CHANNEL

Solid phase extraction pipette

CHROMATOGRAPHY APPARATUS AND METHOD AND MATERIAL FOR MAKING THE SAME

A chromatography apparatus incorporating an improved means for connecting the ligand to the solid support is disclosed. The apparatus comprises a chamber containing a solid support. The solid support is a hydrophobic support. The apparatus includes chromatography surfactants bonded to the solid support. The surfactants comprise a polar group, a hydrophobic functional group substituted on the polar group, and a chromatographic functional group substituted on the polar group. The hydrophobic group is hydrophobically adsorbed to the solid support so that the chromatographic functional group is bound to the solid support and available for binding to compounds which selectively bind thereto. Compositions for and methods of making the foregoing are disclosed. The chromatographic functional group is a ligand for affinity chromatography, an ionogenic group for ion exchange chromatography, or a hydrophobic group for hydrophobic chromatography. Hydrophobic silica particles are preferably used as ...

GAS CHROMATOGRAPH COLUMN WITH CARBON NANOTUBE-BEARING CHANNEL

A carbon nanostructured micro-fabricated gas chromatography column which is particularly well-suited to the surface well-site and/or the downhole analysis of natural gas in oilfield or gasfield applications (but which may also be used in non-oilfield or non-gasfield situations) is described. This micro-fabricated column integrates a micro-structured substrate such as a silicon substrate with carbon nanotubes as an active nanostructured material in a micro-channel. Benefits of the present invention include enhanced separation of alkanes and isomers, particularly below hexane (i.e., below C6), as well as the separation of carbon dioxide, hydrogen sulfide, and water and other substances present in natural gas. The chromatography column of the present invention is in one embodiment a part of an entire gas chromatograph system that in its simplest form also comprises an injector and a detector. Preferably the injector, separation column, and detector are all micro-fabricated on a substrate.

Process and apparatus to deposit a layer of pulverulent substance on the internal walls of capillary tubes or low diameter

METHODS OF MODIFYING A POLYMERIC SURFACE AND PREPARING A MONOLITHIC STATIONARY PHASE, METHODS OF MAKING A CHROMATOGRAPHIC COLUMN SEPARATION AND ASSOCIATED

L'invention se rapporte à un procédé de modification d'une surface d'un support formé en un polymère thermoplastique, qui comprend la préparation d'une composition polymérisable d'ancrage, le dépôt de cette composition polymérisable d'ancrage sur la surface et sa polymérisation par irradiation au moyen de rayons ultraviolets. Selon l'invention, le polymère thermoplastique est transparent à la longueur d'onde des rayons ultraviolets appliqués lors de la polymérisation et la composition polymérisable d'ancrage comprend : - au moins un monomère choisi parmi le diméthacrylate d'éthylène glycol, le diacrylate de 1,4-butanediol, le diméthacrylate de triéthylène glycol et le triméthacrylate de triméthylolpropane, - un ou plusieurs solvants, et - la 2,2-diméthoxy-2-phénylacétophénone. L'invention se rapporte également à un procédé de préparation d'une phase stationnaire monolithique, à un procédé de fabrication d'une colonne de chromatographie comprenant une telle phase stationnaire monolithique ainsi qu'à un procédé de séparation chromatographique mettant en œuvre une telle colonne de chromatographie. The invention relates to a method for modifying a surface of a support formed from a thermoplastic polymer, which comprises preparing a polymerizable anchoring composition, depositing this polymerizable anchoring composition on the surface and its polymerization by irradiation with ultraviolet rays. According to the invention, the thermoplastic polymer is transparent to the wavelength of the ultraviolet rays applied during the polymerization and the polymerizable anchoring composition comprises: - at least one monomer chosen from ethylene glycol dimethacrylate, 1,4-butanediol, triethylene glycol dimethacrylate and trimethylolpropane trimethacrylate, - one or more solvents, and - 2,2-dimethoxy-2-phenylacetophenone. The invention also relates to a process for preparing a monolithic stationary phase, to a process for ...

GAS CHROMATOGRAPHY CAPILLARY DEVICES AND METHODS

A multicapillary bundle for use in a gas chromatograph. Each of the capillaries in the bundle is formed using a coating solution containing a stationary phase and a solvent. The capillaries are coated with stationary phase by reducing pressure at a vacuum end of the capillary and creating a moving interface between the coating solution and a film of stationary phase deposited on each of the capillaries. The reducing pressure at the vacuum end of the capillary and the temperature of the capillary are controlled to maintain motion of the moving interface away from the vacuum end of the capillary. Maintained movement of the interface prevents recoating of the stationary phase. A heating wire and capillaries are embedded in a thermally conductive polymer to create a highly responsive method of heating the multicapillary column. An electronic control device controls the feedback temperature of the multicapillary column using the heating wire.

Deactivated capillary columns for use in capillary electrophoresis

The walls of fused-silica capillary columns used for capillary zone electrophoresis and micellar electrokinetic capillary chromatography may be deactivated with polysiloxanes, polysilazanes and other silicone polymers to permit more effective separations without eliminating electro-osmotic flow within the columns.

Multicapillary column for chromatography and sample preparation

A multicapillary column especially useful for liquid chromatography and sample preparation comprising a plurality of uniform capillaries coated with an insoluble stationary phase, wherein the thickness of the stationary phase is correlated with the radius of the individual capillaries for high efficiency.

SUPPRESSION OF ELECTROOSMOSIS WITH HYDROLYTICALLY STABLE COATINGS

Capillary column

A method and apparatus for manufacturing monolith columns wherein the apparatus comprises a light source 303 and a housing. The method provides a hollow capillary 301 that has internal walls 304 coated with a polymerisable mixture and a light source to a first side of the capillary irradiates the capillary from one side only to effect polymerisation of the polyinerisable material to form a monolith extending inwardly from all internal walls of the capillary. Preferably the light source takes the form of a white fluorescent light wherein the light source and capillary are moveable relative to each other. Advantageously the method and apparatus provides a photo-initiated polymerisation in the generation of porous layer open tubular (PLOT) or full monolith capillary (FMC) columns for separation applications.

SUPPRESSION OF ELECTROOSMOSIS WITH HYDROLYTICALLY STABLE COATINGS

PROCEDURE FOR COATING THE INTERIOR SURFACE OF A REACTION CONTAINER

STRUCTURES SURFACE MODIFIED WITH BIDENTATE SILANES

The invention relates to an improved support comprising a substrate and a bidentate silane attached to the substrate, the bidentate silane containing at least two silicon atoms bridged by certain groups, so arranged that at least a seven-membered ring system is formed in the following manner: where, R1-R4 = alkane, substituted alkane, alkene, substituted alkene, aryl, or substituted aryl: Y = -CH2-, -CH2CH2-, -(CH2)n-, -(CHZ-CHZ)-, or -(CH2)nCHZ-, where Z = alkane, substituted alkane, alkene, substituted alkene, aryl, substituted aryl, halogen, hydroxyl, hydrogen, nitrile, primary, secondary or tertiary or tetralkylamine, carbonyl, carboxyl, amide, sulfonic acid, nitro, nitroso, amide, sulfonamide, etc., n = 1-6, and A are the atoms on the substrate surface to which the silane is covalently attached, which is usefulfor a variety of applications, e.g. chromatographic separations.

AFFINITY SUPPORTS FOR HEMOPERFUSION

A method of coating chromatographic particulate supports to provide a biocompatible outer layer of synthetic membrane-type film which prevents the release of fines but permits the adsorption of components to an affinity ligand is described. The matrix is provided with a membrane-type coating, which prevents leaching of fines, with a pore size of at least 20 angstroms. The coating is applied to a solid particulate under conditions where an integral membrane coat will be formed. It may also be necessary to control the size and number of pores of the membranes by treating a suspension of the solid support in a solvent which contains 0.1-1% of the sugport weight of a biocompatible polymer along with 0.5-5% of the weight of said polymer of a dissolved compatible pore-controlling component. The solvent is then removed from the suspension and the membrane-coated material used in extracorporeal treatment of body fluids or in other chromatographic techniques. The coating process can be conducted before or after the particulate support is functionalized and/or derivatized.

METHOD FOR THE PREPARATION OF MONOLITHIC COLUMNS

A method of preparing a separation column, or channel in a microfabricated device, comprising the steps of: providing an unfilled column, or channel in a microfabricated device; activating the inner wall of the column or channel with an activating agent; filling the column with a polymerization solution comprising a mixture of monomers, at least one porogen and at least one polymerization initiator; and polymerizing the mixture to form a rigid porous monolithic polymer plug in the column or channel. The method is characterized in that that the monomers comprise a mixture of divinylbenzene as major monomer and isodecylacrylate, and that the at least one porogen comprises isobutanol.

MONOLAYER COATING

Monolayer Coating A process for producing a crosslinked, essentially monolayer coating of crosslinked polymer on a substrate, said process consisting of: (a) providing a block copolymer having a first block segment of the general formula: (A)m(B)n wherein A represents a first block segment, B represents a second block segment, m is greater than or equal to 5 molar units, n is greater than or equal to 5 molar units, and at least one of said first block segment and said second block segment contains crosslinkable moieties; (b) introducing said block copolymer into a block selective solvent which is a good solvent for only one of said first block segment or said second block segment, thereby preparing a block copolymer semisolution having a solvated block segment and an essentially nonsolvated block segment; (c) contacting said substrate with said block copolymer semi-solution, thereby producing an essentially monolayer coating on said substrate; and (d) providing activation energy to said ...

METHOD OF MAKING A COLUMN GAS CHROMATOGRAPHY AND COLUMN PRODUCED BY SUCH METHOD

La présente invention se rapporte à un procédé de fabrication d'une colonne de chromatographie, en particulier en phase gazeuse, comprenant une phase stationnaire réalisée à partir d'un sol. Ce procédé comprend les étapes suivantes : (a) l'introduction de ce sol à la première extrémité de la colonne, (b) le déplacement dudit sol en direction de la seconde extrémité de la colonne, de telle sorte qu'une couche de sol se forme sur la paroi interne de la colonne, cette couche étant apte à former un gel sur ladite paroi interne, et (c) le séchage du gel. La présente invention se rapporte également à une colonne capillaire ainsi qu'à une microcolonne susceptibles d'être fabriquées selon ce procédé.

método para a preparação de colunas monolíticas

METHOD FOR COATING THE INTERNAL SURFACE OF A REACTION VESSEL

A method for coating the internal surfaces of a reaction vessel having a small internal diameter comprises the steps of (i) introducing into the reaction vessel a solution of one or more monomers in a suitable solvent; (ii) introducing a flow of an inert gas through the reaction vessel; and (iii) initiating polymerisation of the monomer solution.

APPARATUS AND METHOD OF MULTI-DIMENSIONAL CHEMICAL SEPARATION

A practical way of performing comprehensive multi-dimensional chemical separation using a fist dimension (12) of a two-dimensional chromatograph to generate a chromatogram in a time comparable to or even faster than common practise, while the second dimension (18) generates multiple chromatograms, each in a time comparable to the fastest prior art chromatograph. The transfer of sample portions from the first dimension (12) to the second dimension (18) is through thermal modular inlet stage (14) or by one of several other sample stream modulation techniques, which accumulate portions of sample between the first dimension (12) and the second dimension (18) to transfer them as very sharp concentration pulses analogous to fast injections, without loss of sample and with a substantial improvement in sensitivity.

Micro-miniature gas chromatograph column disposed in silicon wafers

A micro-miniature gas chromatograph column is fabricated by forming matching halves of a circular cross-section spiral microcapillary in two silicon wafers and then bonding the two wafers together using visual or physical alignment methods. Heating wires are deposited on the outside surfaces of each wafer in a spiral or serpentine pattern large enough in area to cover the whole microcapillary area inside the joined wafers. The visual alignment method includes etching through an alignment window in one wafer and a precision-matching alignment target in the other wafer. The two wafers are then bonded together using the window and target. The physical alignment methods include etching through vertical alignment holes in both wafers and then using pins or posts through corresponding vertical alignment holes to force precision alignment during bonding. The pins or posts may be withdrawn after curing of the bond. Once the wafers are bonded together, a solid phase of very pure silicone is injected ...

Multi column chromatography system

The present invention relates to a method and apparatus for chromatographically analyzing each of a plurality of samples in detector, comprising an autosampler to contain a plurality of samples for chromatographic analysis and a pluraltity of chromatographic systems, each system comprising one or more pumps and one or more chromatographic columns. A detector is included for detecting compounds in the samples from each of the chromatography systems along with a valve positioned between the detector and the plurality of chromatography systems, the valve permitting each sample to reach the detector in sequence. A computer control device is included which adjusts the introduction of samples from the autosampler into the plurality of chromatography systems as well as the position of the valve to sequentially separate and deliver compounds within the samples to the detector.

GAS CHROMATOGRAPHY CAPILLARY DEVICES AND METHODS

OPEN TUBULAR CAPILLARIES COMPRISING A CONNECTION LAYER

LIQUID CHROMATOGRAPHY BASED DETECTION AND QUANTITATION OF PHOSPHO PRODRUGS AND THEIR ACTIVE METABOLITES

Способ модификации твердого носителя в хроматографии

Изобретение относитс  к области статического контрол  технологических процессов и воздуха. Целью изобретени   вл етс  ускорение времени модификации сорбентов и удешевление и упрощение процесса приготовлени  сор- . бентов. Подачу пара модификатора на слой твердого сорбента в колонке в потоке газа-носител  осуществл ют при температуре термодинамического равновеси  системы газ - твердое тело. После достижени  равновесного состо ни  при продувке резко снижают температуру колонки с носителем, осажда  пары модификатора на поверхность твердого носител . The invention relates to the field of static control of technological processes and air. The aim of the invention is to accelerate the time of modification of sorbents and reduce the cost and simplify the process of preparation of sor-. bentov. The modifier steam is supplied to the solid sorbent layer in a column in a carrier gas stream at the thermodynamic equilibrium temperature of the gas-solid system. After the equilibrium state is reached, the temperature of the column with the carrier is sharply reduced by blowing, precipitating the modifier pair on the surface of the solid support.

Method for the preparation of monolithic columns

A method of preparing a separation column, or channel in a microfabricated device, comprising the steps of: providing an unfilled column, or channel in a microfabricated device; activating the inner wall of the column or channel with an activating agent; filling the column with a polymerization solution comprising a mixture of monomers, at least one porogen and at least one polymerization initiator; and polymerizing the mixture to form a rigid porous monolithic polymer plug in the column or channel. The method is characterized in that that the monomers comprise a mixture of divinylbenzene as major monomer and isodecylacrylate, and that the at least one porogen comprises isobutanol.

AFFINITY SUPPORTS FOR HEMOPERFUSION

GAS CHROMATOGRAPHY CAPILLARY DEVICES AND METHODS

A multicapillary bundle for use in a gas chromatograph. Each of the capillaries in the bundle is formed using a coating solution containing a stationary phase and a solvent. The capillaries are coated with stationary phase by reducing pressure at a vacuum end of the capillary and creating a moving interface between the coating solution and a film of stationary phase deposited on each of the capillaries. The reducing pressure at the vacuum en d of the capillary and the temperature of the capillary are controlled to maintain motion of th e moving interface away from the vacuum end of the capillary. Maintained movement of the interface prevents recoating of the stationary phase. A heating wire and capillaries are embedd ed in a thermally conductive polymer to create a highly responsive method of heating the multicapillary column. An electronic control device controls the feedback temperature of th e multicapillary column using the heating wire.

SEPARATION SYSTEM, COMPONENTS OF A SEPARATION SYSTEM AND METHODS OF MAKING AND USING THEM

Permeable polymeric monolithic materials are prepared in a column casing. In one embodiment, the permeable polymeric monolithic materials polymerized by the application of heat from an external source starting at a low temperature such as 40 degrees centigrade, depending on the mixture and size of the column, and continuing at a higher temperature, such as 60 degrees centigrade. The temperature at the start of the polymerization is low enough so as not to cause exothermal run-away conditions and to avoid high heat of reaction that would prevent a substantially constant temperature across the cross-section of the column. The higher temperature is used after sufficient monomer depletion has occurred and steric interference has increased so the polymerization reaction is sufficiently slow to avoid heat of reaction generation high enough to cause significant reduction in the homogeneousness of the pore sizes. © KIPO & WIPO 2007 ...

SEPARATION SYSTEM, COMPONENTS OF A SEPARATION SYSTEM AND METHODS OF MAKING AND USING THEM

Permeable polymeric monolithic materials are prepared in a column casing. In one embodiment, the permeable polymeric monolithic materials polymerized by the application of heat from an external source starting at a low temperature such as 40 degrees centigrade, depending on the mixture and size of the column, and continuing at a higher temperature, such as 60 degrees centigrade. The temperature at the start of the polymerization is low enough so as not to cause exothermal run-away conditions and to avoid high heat of reaction that would prevent a substantially constant temperature across the cross-section of the column. The higher temperature is used after sufficient monomer depletion has occurred and steric interference has increased so the polymerization reaction is sufficiently slow to avoid heat of reaction generation high enough to cause significant reduction in the homogeneousness of the pore sizes.

Multicapillary device for sample preparation

A multicapillary sample preparation device, especially useful for handling biological samples, comprising a plurality of uniform capillary tubes coated with a stationary phase, and arranged in a monolithic element. The multicapillary device is suitable for attachment to a pipette, micropipette, syringe, or other analytical or sample preparation instrument.

High efficiency sol-gel gas chromatography column

A capillary column ( 10 ) includes a tube structure having inner walls ( 14 ) and a sol-gel substrate ( 16 ) coated on a portion of inner walls ( 14 ) to form a stationary phase coating ( 18 ) on inner walls ( 14 ). The sol solution used to prepare the sol-gel substrate ( 16 ) has at least one baseline stabilizing reagent and at least one surface deactivation reagent resulting in the sol-gel substrate ( 16 ) having at least one baseling stabilizing reagent residual and at least one surface deactivating reagent residual. A method of making the sol-gel solution is by mixing suitable sol-gel prescursors to form the solution, stabilizing the solution by adding at least one baseline stabilization reagent, deactivating the solution by adding at least one surface deactivation reagent to the solution, and reacting the solution in the presence of at least one catalyst.

Multi column chromatography system

The present invention relates to a method and apparatus for chromatographically analyzing each of a plurality of samples in detector, comprising an autosampler to contain a plurality of samples for chromatographic analysis and a plurality of chromatographic systems, each system comprising one or more pumps and one or more chromatography columns. A detector is included for detecting compounds in the samples from each of the chromatography systems along with a valve positioned between the detector and the plurality of chromatography systems, the valve permitting each sample to reach the detector in sequence. A computer control device is included which adjusts the introduction of samples from the autosampler into the plurality of chromatography systems as well as the position of the valve to sequentially separate and deliver compounds within the samples to the detector.

GAS CHROMATOGRAPH AND METHOD FOR FUNCTIONALIZING SUCH A DEVICE

Dispositif de chromatographie, comprenant un substrat fonctionnel (1), comportant un canal (3) s'étendant entre un premier (3-1) et un deuxième (3-2) orifices débouchant sur une face (5) du substrat fonctionnel ; ladite face (5) du substrat fonctionnel étant disposée contre une face (7) d'un substrat de connexion (9), comportant un troisième (7-1) et un quatrième (7-2) orifices débouchant sur ladite face (7) du substrat de connexion, de sorte que les premier (3-1) et deuxième (3-2) orifices soient disposés respectivement en regard des troisième (7-1) et quatrième (7-2) orifices ; le substrat de connexion étant raccordé à un premier (11) et un deuxième (13) capillaires, le substrat de connexion comportant un premier circuit fluidique (15) s'étendant entre le premier capillaire et le troisième orifice et comportant un deuxième circuit fluidique (17) s'étendant entre le deuxième capillaire et le quatrième orifice ; et un moyen de maintien (19, 21) adapté à maintenir de façon temporaire ladite ...

Freeze drying for gas chromatography stationary phase deposition

The present disclosure relates to methods for deposition of gas chromatography (GC) stationary phases into chromatography columns, for example gas chromatography columns. A chromatographic medium is dissolved or suspended in a solvent to form a composition. The composition may be inserted into a chromatographic column. Alternatively, portions of the chromatographic column may be exposed or filled with the composition. The composition is permitted to solidify, and at least a portion of the solvent is removed by vacuum sublimation.

Separation system, components of a separation system and methods of making and using them

Permeable polymeric monolithic materials are prepared in a column casing. In one embodiment, the permeable polymeric monolithic materials polymerized by the application of heat from an external source starting at a low temperature such as 40 degrees centigrade, depending on the mixture and size of the column, and continuing at a higher temperature, such as 60 degrees centigrade. The temperature at the start of the polymerization is low enough so as not to cause exothermal run-away conditions and to avoid high heat of reaction that would prevent a substantially constant temperature across the cross-section of the column. The higher temperature is used after sufficient monomer depletion has occurred and steric interference has increased so the polymerization reaction is sufficiently slow to avoid heat of reaction generation high enough to cause significant reduction in the homogeneousness of the pore sizes.

Shielded stationary phases

Novel packing materials are provided for liquid chromatography and/or solid phase extraction columns which will allow direct injection of biological fluids. These packing materials have a hydrophilic exterior layer and a hydrophobic, charged or otherwise selective portion that forms an underlayer or is embedded in the hydrophilic layer. During a chromatographic process large water soluble biopolymers will be in contact with the hydrophilic outer layer and be shielded from interacting with the underlayer or embedded portion and elute unretained. Small analytes, on the other hand, can be fully partitioned throughout the exterior and interior layers and are retained by hydrophobic or electrostatic interactions. Using such packings the direct analyses of plasma or serum for drug analysis is demonstrated.

Improvements in gas chromatography

A gas chromatography column comprises a tube containing a longitudinally extended core, the core consisting of, or the core and preferably the inside of the tube being coated with a partitioning agent. In one embodiment the column comprises a capillary tube of internal diameter four to fifty thousandths of an inch and having a wire extending therethrough coated with a partitioning agent. The tube and the core may be of metal, for example copper, gold, nickel, or preferably cupro-nickel, or of polytetrafluoroethylene or nylon. Partitioning agent may be introduced into the column by (a) simple insertion of a coated wire, (b) coating a wire with partitioning agent solution, evaporating the solvent, inserting the wire into a tube and passing therethrough a heated gas to transfer some of the partitioning agent from the wire to the tube, or (c) forcing a partitioning agent solution into the column to coat both wire and tube, and passing a heated gas through the tube to evaporate the solvent. Alternatively the tube may be filled with a liquid or paste, as for example "Araldite" (Registered Trade Mark) which on solidifying contracts to form a core; the core may itself be a partitioning medium, or a partitioning agent may be subsequently introduced directly.

Solid phase extraction pipette

SILICA TRANSFER TUBING

METHOD FOR MEASURING STABLE HEMOGLOBIN A1c USING LIQUID CHROMATOGRAPHY, AND METHOD FOR SIMULTANEOUS MEASUREMENT OF STABLE HEMOGLOBIN A1c AND ABNORMAL HEMOGLOBIN USING LIQUID CHROMATOGRAPHY

The purpose of the present invention is to provide a method for measuring stable hemoglobin A1c in a short time and in a highly reproducible manner, using liquid chromatography. The present invention is a method for measuring stable hemoglobin A1c using liquid chromatography, wherein a filter, the surface of which has been treated with a solution containing 1-50 weight% of silicone oil or a solution containing 1-50 weight% of silicone resin, is placed on the channel of a liquid chromatograph and the pressure generated on the measurement system of the liquid chromatograph is set to 9.8 × 103 Pa to 19.6 × 105 Pa.

Integrated particle trap for capillary plot columns

A porous layer open tubular (PLOT) column includes capillary tubing; one or two particle traps disposed inside one or two end sections of the capillary tubing; and a stationary phase comprising a porous or non-porous material coated inside a main section of the capillary tubing. A method for preparing a porous layer open tubular (PLOT) column includes preparing one or two particle traps inside one or two end sections of a capillary tubing; and preparing a stationary phase comprising a layer of a porous material coated inside a main section of the capillary.

Polyhydrosiloxane compounds and articles and use thereof

The present disclosure, in embodiments, provides a compound of the formula where R¹, R², R³, n, and m are as defined in the specification. The disclosure also provides an article including: a fused silica capillary column treated with a compound of the formula (I), and optionally coated with a stationary phase. The disclosure also provides a separation method, including chromatographing a mixture of compounds on the article.

High efficiency sol-gel gas chromatography column

A capillary column ( 10 ) includes a tube structure having inner walls ( 14 ) and a sol-gel substrate ( 16 ) coated on a portion of inner walls ( 14 ) to form a stationary phase coating ( 18 ) on inner walls ( 14 ). The sol solution used to prepare the sol-gel substrate ( 16 ) has at least one baseline stabilizing reagent and at least one surface deactivation reagent resulting in the sol-gel substrate ( 16 ) having at least one baseline stabilizing reagent residual and at least one surface deactivating reagent residual. A method of making the sol-gel solution is by mixing suitable sol-gel precursors to form the solution, stabilizing the solution by adding at least one baseline stabilization reagent, deactivating the solution by adding at least one surface deactivation reagent to the solution, and reacting the solution in the presence of at least one catalyst.

FUNCTIONALIZED POLYOLEFIN CAPILLARIES FOR OPEN TUBULAR ION CHROMATOGRAPHY

VERFAHREN FÜR DIE CHROMATOGRAPHIE

Romp polymer synthesis

Porous polymer coated capillary chromatographic column as well as preparation method and application thereof

METHODS OF MODIFYING A POLYMERIC SURFACE AND PREPARING A MONOLITHIC STATIONARY PHASE, METHODS OF MAKING A CHROMATOGRAPHIC COLUMN AND SEPARATION THEREOF

L'invention se rapporte à un procédé de modification d'une surface d'un support formé en un polymère thermoplastique, qui comprend la préparation d'une composition polymérisable d'ancrage, le dépôt de cette composition polymérisable d'ancrage sur la surface et sa polymérisation par irradiation au moyen de rayons ultraviolets. Selon l'invention, le polymère thermoplastique est transparent à la longueur d'onde des rayons ultraviolets appliqués lors de la polymérisation et la composition polymérisable d'ancrage comprend : - au moins un monomère choisi parmi le diméthacrylate d'éthylène glycol, le diacrylate de 1,4-butanediol, le diméthacrylate de triéthylène glycol et le triméthacrylate de triméthylolpropane, - un ou plusieurs solvants, et - la 2,2-diméthoxy-2-phénylacétophénone. L'invention se rapporte également à un procédé de préparation d'une phase stationnaire monolithique, à un procédé de fabrication d'une colonne de chromatographie comprenant une telle phase stationnaire monolithique ainsi qu'à un procédé de séparation chromatographique mettant en œuvre une telle colonne de chromatographie. The invention relates to a method for modifying a surface of a support formed from a thermoplastic polymer, which comprises preparing a polymerizable anchoring composition, depositing this polymerizable anchoring composition on the surface and its polymerization by irradiation with ultraviolet rays. According to the invention, the thermoplastic polymer is transparent to the wavelength of the ultraviolet rays applied during the polymerization and the polymerizable anchoring composition comprises: - at least one monomer chosen from ethylene glycol dimethacrylate, 1,4-butanediol, triethylene glycol dimethacrylate and trimethylolpropane trimethacrylate, - one or more solvents, and - 2,2-dimethoxy-2-phenylacetophenone. The invention also relates to a process for preparing a monolithic stationary phase, to a process for ...

METHOD OF MAKING A COLUMN GAS CHROMATOGRAPHY AND COLUMN PRODUCED BY SUCH METHOD

GAS CHROMATOGRAPHY DEVICE AND METHOD OF FUNCTIONALIZING SUCH A DEVICE

METHOD FOR THE PREPARATION OF MONOLITHIC COLUMNS

A method of preparing a separation column, or channel in a microfabricated device, comprising the steps of: providing an unfilled column, or channel in a microfabricated device; activating the inner wall of the column or channel with an activating agent; filling the column with a polymerization solution comprising a mixture of monomers, at least one porogen and at least one polymerization initiator; and polymerizing the mixture to form a rigid porous monolithic polymer plug in the column or channel. The method is characterized in that that the monomers comprise a mixture of divinylbenzene as major monomer and isodecylacrylate, and that the at least one porogen comprises isobutanol.

COMPREHENSIVE 2DGC SYSTEM COMPRISING OF A MODULATION COLUMN, A MODULATOR, AND A GAS CHROMATOGRAPH

A comprehensive two-dimensional gas chromatography system comprising of a sample inlet, a primary dimension column, a secondary dimension column, a thermal modulator, and a detector. The thermal modulator has a first modulation position and a second modulation position. The sample inlet connects to the primary dimension column. The exit of the primary dimension column connects to the first modulation position via a fluidic path, the first modulation position connects to the second modulation position via a fluidic path, the second modulation position connects to the secondary dimension column via a fluidic path, and the exit of the secondary dimension column connects to the detector. The fluidic path between the exit of the primary dimension column and the inlet of the secondary dimension column is a modulation column. 1. A modulation column used in a comprehensive two-dimensional gas chromatography system: the modulation column has only part of its length coated with a stationary phase. The modulation column is either an independent part from the primary dimension column and the secondary dimension column , or an integral part of the primary dimension column or the secondary dimension column.2. The modulation column of claim 1 , has a first and a second modulation positions claim 1 , wherein (1) only the first and second modulation positions have stationary phase coating; or (2) only the first modulation position has stationary phase coating; or (3) only the first modulation position and a distance extending to its upstream has stationary phase coating; or (4) only the first modulation position claim 1 , the second modulation position claim 1 , and the length between these two positions have stationary phase coating; or (5) only the first modulation position claim 1 , the second modulation position claim 1 , the length between these two positions claim 1 , and a distance extending to upstream of the first modulation position have stationary phase coating; or (6) ...

Methods and apparatus for making a chromatography column

Methods for depositing a stationary phase in a tube for chromatography. The resulting column may be a variable gradient column or a standard open tubular column with a uniform thickness stationary phase. The methods include providing a tube comprising an electrically conductive interior surface and having a composition within the tube, the composition comprising a stationary phase precursor and at least one of an electrolyte and a reactant precursor, and electrochemically reacting the reactant precursor or the stationary phase precursor to form a stationary phase in the tube.

Multi column chromatography system

The present invention relates to a method and apparatus for chromatographically analyzing each of a plurality of samples in detector, comprising an autosampler to contain a plurality of samples for chromatographic analysis and a plurality of chromatographic systems, each system comprising one or more pumps and one or more chromatography columns. A detector is included for detecting compounds in the samples from each of the chromatography systems along with a valve positioned between the detector and the plurality of chromatography systems, the valve permitting each sample to reach the detector in sequence. A computer control device is included which adjusts the introduction of samples from the autosampler into the plurality of chromatography systems as well as the position of the valve to sequentially separate and deliver compounds within the samples to the detector.

PLOT-Säulen für die Gaschromatographie sowie Verfahren und Vorrichtung zu deren Herstellung

PLOT-Säule für die Gaschromatographie aus einer Quarzglaskapillare, deren Innenfläche eine Schicht aufgewachsener MOF-Kristallite aufweist, dadurch gekennzeichnet, dass die Innenfläche mit Spacermolekülen modifziert ist, wobei die Spacermoleküle mittels einer Ankergruppe mit der Innenfläche der Quarzglaskapillare und mittels einer Kopfgruppe mit den MOF-Kristalliten so verbunden sind, dass die Kopfgruppen an den der Innenfläche zugewandten Metalloxidclustern der MOF-Kristallite binden.

Suppression of electroosmosis with hydrolytically stable coatings

Solid phase extraction pipette

Solid phase extraction devices for sample preparation are disclosed, comprising a hollow conical tube having one narrower opening and one broader opening, wherein the narrower opening of the tube contains a solid phase extraction material comprising a functionalized monolithic sorbent, and wherein the solid phase extraction device is prepared by a combination of reduced pressure, positive pressure and mechanical compaction. The solid phase extraction devices are adapted for preparation of small sample volumes, and provide excellent recovery of analytes and good flow characteristics. Methods for preparing and using the solid phase extraction devices are disclosed.

SUPPRESSION OF ELECTROOSMOSIS WITH HYDROLYTICALLY STABLE COATINGS

METAL COMPONENTS WITH INERT VAPOR PHASE COATING ON INTERNAL SURFACES

Patent Application Atty Docket No. 20120138-02 Abstract The invention provides metal liquid chromatography components with uniformly coated internal surfaces and methods for achieving the same. The invention addresses the problem of corrosion or interference of metal components in the flow path for LC analyses in which the sample interacts with metal ions or surfaces. The invention also alleviates the difficulties in coating very long metal tubes and very small metal channels with an inert, continuous coating that adheres well to metal surfaces. The metal flow path is rendered inert by the coating, and thus compatible with bioanalytical separations, for example, by using a vapor phase deposition process to coat the inner surfaces with a coating that continuously covers all metal surfaces in the flow path. Patent Application Atty Docket No. 20120138-02 FIG. 1. Schematic illustration of an exemplary embodiment of the invention with dual layers of coatings ...

MICROWAVE-ASSISTED CHROMATOGRAPHY PREPARATION

An instrument and associated method are disclosed for preparing samples for column chromatography. The method includes the steps of applying microwave energy to a sample composition containing at least one solvent to encourage a chemical reaction and generate desired products, thereafter mixing an absorbent media with the sample to absorb the solvent, the media being compatible with liquid chromatography that will separate the expected products, being chemically inert to the expected products, and being added in an amount sufficient to provide a substantially dry mixture of the media and the sample, but less than an amount that overly broadens the resolution of the sample during liquid chromatography, thereafter applying microwave energy to the dry mixture of the media and the sample to thereby encourage the solvent to evaporate under the influence of the microwave energy, and thereafter adding the dry mixture of the media and the remaining sample to a liquid chromatography column and separating ...

SEPARATION SYSTEM, COMPONENTS OF A SEPARATION SYSTEM AND METHODS OF MAKING AND USING THEM

A method to cover to a solid surface, bearing exposed silanols groups, for decreasing the présencede their electrostatic loads, and application to the protein separation

Procédé pour revêtir une surface solide, portant des groupes silanols exposés, pour diminuer la présence de leurs charges électro-statiques, et application à la séparation de protéines. On applique une couche de revêtement, stable à l'hydrolyse, en transformant les groupes silanols de la surface solide en des groupes halogénures de silicium, que l'on fait ensuite réagir avec un réactif organométallique comportant un fragment éthényle terminal pour obtenir des groupes Si-R (R conservant le fragment éthényl terminal) et en faisant ensuite reagir ces groupes éthényles avec un monomère organique, neutre, par polymérisation d'addition, pour former sur la surface à protéger une couche monomoléculaire de polymère non réticulé La couche de polymère, reliée directement, est stable dans une large gamme de pH. Application: traitement des parois intérieures de tubes capillaires en silice (fondue) pour des séparations par chromatographie et électrophorèse. Process for coating a solid surface, bearing exposed silanol groups, to decrease the presence of their electrostatic charges, and application to the separation of proteins. A coating layer, stable to hydrolysis, is applied by transforming the silanol groups of the solid surface into silicon halide groups, which is then reacted with an organometallic reagent comprising a terminal ethenyl moiety to obtain Si groups. -R (R retaining the terminal ethenyl moiety) and then reacting these ethenyl groups with an organic, neutral monomer, by addition polymerization, to form on the surface to be protected a monomolecular layer of uncrosslinked polymer The polymer layer, directly linked, is stable over a wide pH range. Application: treatment of the inner walls of capillary tubes in silica (fused) for separations by chromatography and electrophoresis.

CHROMATOGRAPHIC TECHNIQUE AND APPARATUS

A compact, sensitive, comprehensive two-dimensional gas chromatographic system (10) includes a chromatrographic column (14) having first section (14A) and second section (14B) in series with each other to permit the flow of sample (12) and a carrier (13) through the sections. The retention time of second section (14B) is less than the band resolution time of first section (14A). To control the wave fronts between the sections, first heater (22) and second heater (26) are positioned to heat and drive off sample collected at the outlet of first section (14A) for collection in second section (14B) and to heat sample collected at the inlet of second section (14B) so that first heater (22) rapidly drives off sample for collection in second section (14B) and then second section (14B) rapidly drives off sample in sharp wave front while first section (14A) is accumulating another band of later movement into second section (14B).

Micro Circulatory Gas Chromatography System and Method

A gas chromatography system can include a circulatory loop, a gas inlet positioned along the circulatory loop, a gas outlet positioned along the circulatory loop, a micro column positioned in line with the circulatory loop, and an in-line population sensor positioned in line with the circulatory loop. The in-line population sensor can be configured to detect changes in gas population. The gas inlet and gas outlet can be associated with a gas inlet valve and gas outlet valve, and configured to admit or withdraw gas from the circulatory loop, respectively. A gas sample can be circulated through the circulatory loop for at least one cycle, and a component of the gas sample can be detected using the in-line population sensor.

Ion chromatography system for exchanging an ion exchanger in a suppressor and a suppressor means

Suppression of electroosmosis with hydrolytically stable coatings

Surfaces of silica-containing materials, such as the inner walls of silica capillaries, used in chromatographic, particularly electrophoretic, separations are coated with an organic polymer layer to reduce or eliminate surface charges. The layer is applied by first converting the silanol groups on the surface to silicon halide groups, then reacting these groups with an organometallic reagent having a terminal ethenyl moiety, preferably vinyl or allyl lithium or a vinyl or allyl magnesium halide, to convert the silicon halide groups to Si-R groups where the R retains the terminal ethenyl moiety, and finally reacting these ethenyl groups newly attached to the surface with a neutral organic monomer in an addition polymerization reaction to form a monomolecular noncrosslinked polymer layer over the surface. The resulting polymer layer is linked to the silica directly through a Si-C bond which is stable over a wide range of pH conditions.

Capillary column and method of making

MULTI COLUMN CHROMATOGRAPHY SYSTEM

The present invention relates to a method and apparatus for chromatographically analyzing each of a plurality of samples in detector, comprising an autosampler to contain a plurality of samples for chromatographic analysis and a plurality of chromatographic systems, each system comprising one or more pumps and one or more chromatography columns. A detector is included for detecting compounds in the samples from each of the chromatography systems along with a valve positioned between the detector and the plurality of chromatography systems, the valve permitting each sample to reach the detector in sequence. A computer control device is included which adjusts the introduction of samples from the autosampler into the plurality of chromatography systems as well as the position of the valve to sequentially separate and deliver compounds within the samples to the detector.

OPEN TUBULAR CAPILLARIES HAVING A CONNECTING LAYER

The invention relates to a method for producing open tubular capillaries containing monolithic sorbents and to said capillaries. The inventive capillaries are characterised by a connection layer between the capillary wall and the sorbent, said layer ensuring a particularly good adhesion of the sorbent to the capillary wall.

Separation system, components of a separation system and methods of making and using them

The invention is related to a method of making a monolithic chromatography column comprising the steps of adding a polymerization mixture containing a porogen to a closed container, polymerizing the mixture under pressure to form a polymer plug whereby sufficient pressure is applied to prevent voids being formed caused by vacuum due to shrinkage during polymerization mixture to a controlled elevated temperature, and washing the polymer plug to remove the porogen.

POLYMER RETENTION SCREENING METHOD

A method and apparatus for depositing a coating on the internal walls of capillary or smallbore tubes

... 1,088,421. Tubes coated with reagents; blood sedimentation rate tests. HARSHAW CHEMICALS Ltd. Dec. 29, 1964 [Jan. 7, 1964], No. 716/64. Heading B1X. [Also in Division B6] Capillary or small-bore glass tubes are provided with an internal uniform coating of powdered material by inserting a quantity of the powder 30 and a plurality of the tubes in each of two glass cylinders 24, 25 which are then coupled together by a threaded member 26 to which is secured a metal screen 27 through which the powder, but not the tubes, can pass, mounting the assembly at an angle to the horizontal, by means of rubber bands 20, on a wooden stand 14, and vibrating the assembly by means of a band of animal fur 13 having an enlargement 28 and mounted on a driven pulley 12 mounted obliquely so that the impact of the enlargement 28 on the assembly vibrates it and also causes it to rotate about its axis. Contact of the powder with the tubes, and also of the fur with the cylinders, produces an electrostatic charge which ...

Zeolitic capillary columns for gas chromatography

Methods have been found to prepare fused silica capillary gas chromatographic columns where the stationary phase is a molecular sieve affixed to the silica capillary wall without the aid of an organic binder by modifying the interior surface of the silica prior to contact with the molecular sieve. These totally inorganic columns greatly expand the application and range of gas chromatographic separations and allow the use of non-traditional carrier gases, even air, while not degrading the separation of components. The columns are films of small molecular sieve particles affixed to a silica surface modified by such treatments as hydrogen peroxide, alumina deposition, or silica deposition followed by fixation at 80°-160° C.

Ion chromatography system for exchanging an ion exchanger in a suppressor and a suppressor means

LOW BINDING SURFACES FOR PEPTIDE MAPPING

The present disclosure discusses a method of separating a sample (e.g., peptide compound) including coating a flow path of a chromatographic system; injecting the sample into the chromatographic system; flowing the sample through the chromatographic system; separating the sample; and analyzing the separated sample. In some examples, the coating applied to the surfaces defining the flow path is non-binding with respect to the sample – and the separated sample. Consequently, the sample does not bind to the low-binding surface of the coating (e.g., organosilica coating) of the flow path. The applied coating can reduce peak tailing and increase analyte recovery for the sample of the chromatographic system.

Joining by coating components

A method of making a fluid conduit 290 for high performance liquid chromatography from two components 200 & 250, each having a coating 230 & 260 on a side thereof and at least one of these sides having an indentation therein. At least one coating 230,260 is activated by means of ion bombardment, plasma treatment, corona discharge ion beam treatment, atom bombardment, etching or UV or passivation is inhibited. The coated sides of the components 200,250 are pressed together to form a body in which the conduit 290 lies either parallel to or perpendicular to the abutting sides of the components 200,250. The coatings 230,260 can be PVD or CVD deposited diamond-like carbon which can be doped (e.g. by O, Si, N or fluorinated DLC), a ceramic, a carbide (e.g. BTiC), titanium nitride, Ti2AlN or silicon. Each component 200,250 can further comprise an intermediate adhesion layer. The method can be used to coat and bond together components made from metal sheet (e.g stainless steel), polymers (e.g.

Capillary column and method of making

SEPARATION SYSTEM, COMPONENTS OF A SEPARATION SYSTEM AND METHODS OF MAKING AND USING THEM

Permeable polymeric monolithic materials are prepared in a column casing. In one embodiment, the permeable polymeric monolithic materials polymerized by the application of heat from an external source starting at a low temperature such as 40 degrees centigrade, depending on the mixture and size of the column, and continuing at a higher temperature, such as 60 degrees centigrade. The temperature at the start of the polymerization is low enough so as not to cause exothermal run-away conditions and to avoid high heat of reaction that would prevent a substantially constant temperature across the cross-section of the column. The higher temperature is used after sufficient monomer depletion has occurred and steric interference has increased so the polymerization reaction is sufficiently slow to avoid heat of reaction generation high enough to cause significant reduction in the homogeneousness of the pore sizes.

Multi column chromatography system

The present invention relates to a method and apparatus for chromatographically analyzing each of a plurality of samples in detector, comprising an autosampler to contain a plurality of samples for chromatographic analysis and a plurality of chromatographic systems, each system comprising one or more pumps and one or more chromatography columns. A detector is included for detecting compounds in the samples from each of the chromatography systems along with a valve positioned between the detector and the plurality of chromatography systems, the valve permitting each sample to reach the detector in sequence. A computer control device is included which adjusts the introduction of samples from the autosampler into the plurality of chromatography systems as well as the position of the valve to sequentially separate and deliver compounds within the samples to the detector.

Multicapillary column for chromatography and sample preparation

A multicapillary column especially useful for liquid chromatography and sample preparation comprising a plurality of uniform capillaries coated with an insoluble stationary phase, wherein the thickness of the stationary phase is correlated with the radius of the individual capillaries for high efficiency.

Säulenfüllung für Flüssigkeits-Chromatographie, Trennsäule und Flüssigkeits-Chromatographie-Gerät

Eine Säulenfüllung, eine Trennsäule, ein Analysegerät und ein Analyseverfahren werden bereitgestellt, die eine Analysezeit verkürzen, ohne die Abscheideleistung von multi-komponenten-Aminosäuren zu verschlechtern. Offenbart wird eine Säulenfüllung, die einen Kernbereich aus einem Styrol-Di-Vinylbenzol-Copolymer mit einem Vernetzungsgrad von 50% und eine Außenhaut aus Styrol-Di-Vinylbenzol-Copolymer mit einem Vernetzungsgrad von 20% oder weniger umfasst; eine die Säulenfüllung nutzende Trennsäule sowie ein Hochgeschwindigkeits-Flüssigkeitschromatographiegerät und ein Analyseverfahren, welche diese Trennsäule nutzen.

Solid phase extraction pipette

Microwave-assisted chromatography preparation

An instrument and associated method are disclosed for preparing samples for column chromatography. The method includes the steps of applying microwave energy to a sample composition containing at least one solvent to encourage a chemical reaction and generate desired products, thereafter mixing an absorbent media with the sample to absorb the solvent, the media being compatible with liquid chromatography that will separate the expected products, being chemically inert to the expected products, and being added in an amount sufficient to provide a substantially dry mixture of the media and the sample, but less than an amount that overly broadens the resolution of the sample during liquid chromatography, thereafter applying microwave energy to the dry mixture of the media and the sample to thereby encourage the solvent to evaporate under the influence of the microwave energy, and thereafter adding the dry mixture of the media and the remaining sample to a liquid chromatography column and separating ...

System for preparing packed columns and coated capillary tubes useful in gas chromatography

An integral system contained in a suitable housing which includes means for coating particulate support material with stationary phase chemicals, means for draining liquid from the coated support material, means for drying the coated support material, and means for transferring the dried, coated support material into a gas-chromatography column. Means for cleaning and coating capillary tubes is also disclosed. Additionally means for conditioning packed columns and capillary tubes is disclosed.

Multi column chromatography system

The present invention relates to a method and apparatus for chromatographically analyzing each of a plurality of samples in detector, comprising an autosampler to contain a plurality of samples for chromatographic analysis and a plurality of chromatographic systems, each system comprising one or more pumps and one or more chromatography columns. A detector is included for detecting compounds in the samples from each of the chromatography systems along with a valve positioned between the detector and the plurality of chromatography systems, the valve permitting each sample to reach the detector in sequence. A computer control device is included which adjusts the introduction of samples from the autosampler into the plurality of chromatography systems as well as the position of the valve to sequentially separate and deliver compounds within the samples to the detector.

Method for coating the internal surface of a reaction vessel

A method for coating the internal surfaces of a reaction vessel having a small internal diameter comprises the steps of (i) introducing into the reaction vessel a solution of one or more monomers in a suitable solvent; (ii) introducing a flow of an inert gas through the reaction vessel; and (iii) initiating polymerization of the monomer solution.

METHOD FOR COVALENTLY ATTACHING POLYMERIC MONOLITHS TO POLYETHER ETHER KETONE (PEEK) SURFACES

Method for covalently attaching polymeric monoliths to polyether ether ketone (PEEK) surfaces The present invention provides a method of covalently attaching a polymeric monolith to the internal surface of polyether ether ketone (PEEK) tubing and column housings, comprising the steps of: (a) reducing the ketone group of the PEEK to a hydroxyl group to obtain a modified PEEK, (b) optionally reacting the hydroxyl group obtained in step (a) with a compound having an active vinyl group to form a modified PEEK selected from the group of acrylate modified PEEK, methacrylate modified PEEK, styrene modified PEEK and epoxy modified PEEK, and (c) reacting the modified PEEK obtained in step (a) or (b) with a polymer or polymerization mixture for forming the polymeric monolith. Hereby, the mechanical stability and solvent durability of larger diameter monolithic columns as well as their overall performance are improved.

Method of making ionic liquid mediated sol-gel sorbents

Ionic liquid (IL)-mediated sol-gel hybrid organic-inorganic materials present enormous potential for effective use in analytical microextraction. One obstacle to materializing this prospect arises from high viscosity of ILs significantly slowing down sol-gel reactions. A method was developed which provides phosphonium-based, pyridinium-based, and imidazolium-based IL-mediated advanced sol-gel organic-inorganic hybrid materials for capillary microextraction. Scanning electron microscopy results demonstrate that ILs can serve as porogenic agents in sol-gel reactions. IL-mediated sol-gel coatings prepared with silanol-terminated polymers provided up to 28 times higher extractions compared to analogous sol-gel coatings prepared without any IL in the sol solution. This study shows that IL-generated porous morphology alone is not enough to provide effective extraction media: careful choice of the organic polymer and the precursor with close sol-gel reactivity must be made to ensure effective chemical bonding of the organic polymer to the created sol-gel material to be able to provide the desired sorbent characteristics.

Metal components with inert vapor phase coating on internal surfaces

The invention provides metal liquid chromatography components with uniformly coated internal surfaces and methods for achieving the same. The invention addresses the problem of corrosion or interference of metal components in the flow path for LC analyses in which the sample interacts with metal ions or surfaces. The invention also alleviates the difficulties in coating very long metal tubes and very small metal channels with an inert, continuous coating that adheres well to metal surfaces. The metal flow path is rendered inert by the coating, and thus compatible with bioanalytical separations, for example, by using a vapor phase deposition process to coat the inner surfaces with a coating that continuously covers all metal surfaces in the flow path.

Use of vapor deposition coated flow paths for improved chromatography of metal interacting analytes

R1, R2, R3, R4, R5, and R6 are each independently selected from (C1-C6)alkoxy, —NH(C1-C6)alkyl, —N((C1-C6)alkyl)2, OH, ORA, and halo. RA represents a point of attachment to the interior surfaces of the fluidic system. At least one of R1, R2, R3, R4, R5, and R6 is ORA. X is (C1-C20)alkyl, —O[(CH2)2O]1-20—, —(C1-C10)[NH(CO)NH(C1-C10)]1-20-, or —(C1-C10)[alkylphenyl(C1-C10)alkyl]1-20-.

Liquid chromatography technique

LC techniques are disclosed. The LC technique includes providing a liquid chromatography system having a coated metallic fluid-contacting element, and transporting a fluid to contact the coated metallic fluid contacting element. Conditions for the transporting of the fluid are selected from the group consisting of the temperature of the fluid being greater than 150 degree Celsius, pressure urging the fluid being greater than 60 MPa, the fluid having a protein-containing analyte incompatible with one of titanium and polyether ether ketone, the fluid having a chelating agent incompatible with the one or both of the titanium or the polyether ether ketone.

LOW POLLUTANT DIALYSIS SOLUTION

The present invention relates to a method for determination of pollutants and leachables in dialysis solutions by stir bar sorptive extraction comprising the steps of 1. Method for determination of pollutants and leachables in dialysis solutions by stir bar sorptive extraction comprising the steps ofa. Conditioning of the stir bar coated with a sorptive materialb. Stirring the dialysis solution with a coated stir barc. Desorption of pollutants and leachables from the coated stir bar.2. Method of further comprising the step ofd. Analysis of the pollutants and leachables by GC-MS.3. Method of claim 1 , wherein the conditioning step a) comprises washing in a mixture comprising methanol and dichloromethane.4. Method of claim 3 , wherein the conditioning step a) additionally comprises ultrasonic treatment.5. Method of claim 1 , wherein the sorptive material claim 1 , of the stir bar is poly-dimethylsiloxane (PDMS).6. A process for validating a batch of a dialysis solution in a polymer container comprising the steps of{'claim-ref': {'@idref': 'CLM-00001', 'claim 1'}, 'a. determining the total amount of diethyl phthalate or dibutyl phthalate in a sample of the batch after heat sterilization by the method according to , and'}b. validating the batch for distribution only if the sample of the batch is determined in step a) to contain less than 150 ng/L by weight of a leachable or pollutant.7. The process of claim 6 , wherein the batch is validated for distribution only if the sample of the batch is determined in step a) to contain less than 150 ng/L of diethylphthalate or dibutyl phthalate.8. The process of claim 7 , wherein the batch is validated for distribution only if the sample of the batch is determined in step a) to contain less than 100 ng/L of diethylphthalate or dibutylphthalate.9. Process for validating primary packaging material for dialysis solutions comprising the steps of:a. filling a dialysis solution in a primary packaging material,b. heat sterilizing the ...

USE OF VAPOR DEPOSITION COATED FLOW PATHS FOR IMPROVED CHROMATOGRAPHY OF METAL INTERACTING ANALYTES

A chromatographic device including a coated metallic frit is disclosed. The coating is provided over the fluid exposed surfaces of the frit, thereby covering metallic surfaces to prevent interaction with an analyte in the flowstream. This technology relates to the use of vapor deposition coated frit(s) in a liquid flow path for improved chromatography. More specifically, this technology relates to liquid chromatographic devices for separating analytes in a sample having coated frit(s) within an uncoated metallic fluidic flow path (i.e., the column tube or channel is formed of stainless steel, titanium (pure or alloyed), or some mixture of stainless steel and titanium) and does not include the coating applied to the frit. 1. A chromatographic column , comprising:an uncoated tube comprising stainless steel or titanium or both; anda coated frit comprising a coating, wherein the coated frit is disposed proximate to an inlet of the tube,wherein the uncoated tube does not have the coating, andthe coating reduces binding of one or more sample components to the coated frit relative to binding of the one or more sample components to the uncoated tube.2. The chromatographic column of claim 1 , wherein the coating is an organosilica.3. The chromatographic column of claim 2 , wherein the organosilica comprises an alkylsilyl.5. The chromatographic column of claim 1 , further comprising a second coated frit disposed within the uncoated tube.6. The chromatographic column of claim 1 , wherein the coated frit includes an underlying substrate of stainless steel.7. The chromatographic column of claim 1 , wherein the coated frit includes an underlying substrate of titanium.8. The chromatographic column of claim 1 , wherein the uncoated tube has a length to diameter ratio of between 40 and 4.9. The chromatographic column of claim 1 , wherein the coating has a thickness of at least 100 Å.10. The chromatographic column of claim 4 , wherein a vapor reagent used to form coating is bis( ...

LIQUID CHROMATOGRAPHY TECHNIQUE

Liquid chromatography techniques are disclosed. Specifically, the liquid chromatography technique includes providing a liquid chromatography system having a coated metallic fluid-contacting element, and transporting a fluid to contact the coated metallic fluid-contacting element. Conditions for the transporting of the fluid are selected from the group consisting of the temperature of the fluid being greater than 150° C., pressure urging the fluid being greater than 60 MPa, the fluid having a protein-containing analyte incompatible with one or both of titanium and polyether ether ketone, the fluid having a chelating agent incompatible with the one or both of the titanium or the polyether ether ketone, and combinations thereof 1. A liquid chromatography technique , comprising:providing a liquid chromatography system having a coated stainless steel fluid-contacting element; andtransporting a fluid to contact the coated stainless steel fluid-contacting element;wherein the fluid includes adenosine triphosphate;wherein the coated stainless steel fluid-contacting element has a coating, the coating including carbon, silicon, oxygen, and hydrogen.2. The technique of claim 1 , wherein the coated stainless steel fluid-contacting element is a frit.3. The technique of claim 1 , wherein the coated stainless steel fluid-contacting element is a fitting.4. The technique of claim 1 , wherein the coated stainless steel fluid-contacting element is a pump head.5. The technique of claim 1 , wherein the coated stainless steel fluid-contacting element is a valve.6. The technique of claim 1 , wherein the liquid chromatography system has a stationary phase claim 1 , the stationary phase having particles having a size of less than 6 micrometers.7. The technique of claim 1 , wherein the liquid chromatography system has a stationary phase claim 1 , the stationary phase having particles being hydrophobic.8. The technique of claim 1 , wherein the liquid chromatography system includes a solvent ...

METHOD FOR MANUFACTURING A GAS PHASE CHROMATOGRAPHY COLUMN AND COLUMN OBTAINED USING SUCH A METHOD

The present invention relates to a method for manufacturing a chromatography column, in particular for a gas phase chromatography, comprising a stationary phase made from a sol. 1. A method for manufacturing a chromatography column comprising a stationary phase made from a sol comprising a pore-forming agent , comprising:(a) introducing a sol comprising a pore-forming agent at a first end of the column,(b) moving said sol towards a second end of the column, so that a sol layer is formed on the internal wall of the column wherein said sol layer forms a gel on the internal wall of the column, and(c) drying the gel, and(d) removing the pore-forming agent from the dried layer, so as to form a microporous, mesoporous layer or other porous layer, the size and/or the density of the pores being controlled, said porous layer forming the stationary phase.2. The method according to claim 1 , wherein the sol forms a plug claim 1 , extending from the first end of the column and over a length of less than two-thirds of the total length of the column claim 1 , the plug being moved along the column under the effect of a pressure.3. The method according to claim 1 , wherein (c) is carried out by circulating a gas inside the column and claim 1 , if required claim 1 , during (a).4. The method according to claim 2 , wherein the gas is air or helium claim 2 , nitrogen or another inert gas.5. The method according to claim 1 , wherein the pore-forming agent comprises cetyltrimethylammonium bromide (CTAB) claim 1 , diblock copolymers of ethylene oxide and of propylene oxide claim 1 , triblock copolymers of ethylene oxide and of propylene oxide claim 1 , or another surfactant.6. The method according to claim 1 , wherein (d) is carried out after (c) with a treatment selected from the group consisting of calcination claim 1 , washing with an organic solvent of the alcohol or acetone type claim 1 , and UV insolation.7. The method according to claim 6 , wherein the calcination is carried out by ...

USE OF VAPOR DEPOSITION COATED FLOW PATHS FOR IMPROVED ANALYTICAL ANALYSIS

A device for processing samples is disclosed. Interior surfaces of the device, which come in contact with fluids, define wetted surfaces. A portion of the wetted surfaces are coated with an alkylsilyl coating having the Formula I: 2. The sample preparation device of claim 1 , wherein a material forming the wetted surfaces of the fluidic path prior to coating are formed of a polymeric material.3. The sample preparation device of claim 1 , wherein a material forming the wetted surfaces of the fluidic path prior to coating are formed of glass.4. The sample preparation device of claim 1 , wherein a material forming the wetted surfaces of the fluidic path prior to coating are formed of metal.5. The sample preparation device of claim 1 , wherein the alkylsilyl coating has a contact angle of at least 15°.6. The sample preparation device of claim 5 , wherein the alkylsilyl coating has a contact angle of less than or equal to 60°7. The sample preparation device of claim 1 , wherein the alkylsilyl coating has a thickness of at least 100 Å.8. The sample preparation device of claim 1 , wherein the alkylsilyl coating of Formula I is bis(trichlorosilyl)ethane or bis(trimethoxysilyl)ethane.10. The sample preparation device of claim 9 , wherein the alkylsilyl coating of Formula II is (3-glycidyloxypropyl)trimethoxysilane claim 9 , n-decyltrichlorosilane claim 9 , trimethylchlorosilane claim 9 , trimethyldimethyaminosilane claim 9 , methoxy-polyethyleneoxy(1-10) propyl trichlorosilane claim 9 , or methoxy-polyethyleneoxy (1-10) propyl trimethoxysilane.11. The sample preparation device of claim 10 , wherein the alkylsilyl coating of Formula II is (3-glycidyloxypropyl)trimethoxysilane followed by hydrolysis.12. The sample preparation device of claim 9 , wherein the alkylsilyl coating of Formula I and II provides a desired contact angle of about 5° to about 60°.13. The sample preparation device of claim 9 , wherein the alkylsilyl coating of Formula I is bis(trichlorosilyl)ethane or bis ...

Chromatography method

Method for exchanging materials, wherein a gaseous, liquid or supercritical mobile phase containing species to be separated is circulated through a packing comprising a stationary phase, the method being characterised in that:—the packing comprises a plurality of capillary ducts formed in at least one first material, the ducts passing through the packing between an upstream face through which the mobile phase enters the packing and a downstream face through which the mobile phase leaves the packing,—each duct comprises, on at least one portion of the inner wall thereof, at least one secondary material consisting of an organic gel or porous mineral,—the thickness of the secondary material defines, inside the duct, at least one empty tubular channel of solid material, the channel being open so as to allow the mobile phase to enter and extending continuously between the upstream and downstream faces of the capillary duct—the secondary material has a thickness between 0.05 times and 0.5 times the diameter of the channel—the method is carried out with a velocity of the mobile phase between 5.0 times and 50 times the speed of the optimum mobile phase defined by the minimum of the Van Deemter curve of the majority separating compound under the method conditions—the cumulative volume of the capillary ducts is more than 15% of the total packing volume.

GC-FTIR and Mode of Operation to Address Water Interference

Samples are analyzed in a system that includes a gas chromatography column for separating components in a sample and a spectrometry system for detecting these components. An interferent present in the sample, water for example, flows through the column and the sample cell of the spectrometry system before beginning the analysis of analytes. 1. An analysis method comprising:allowing a fluid interferent from an interferent-containing sample to flow through a gas chromatography column and a sample cell of a spectrometry system before beginning an analysis of analytes.2. The method of claim 1 , wherein a flow rate of another carrier fluid added to the fluid interferent is within the range of from 0 mL/min to about 0.5 mL/min.3. The method of claim 1 , wherein another carrier gas is added to the fluid interferent at a flow rate sufficient to prevent back flow of the fluid interferent claim 1 ,4. The method of claim 1 , wherein a flow rate of another carrier fluid added to the fluid interferent is no greater than about 5% relative to the flow rate of the fluid interferent.5. The method of claim 1 , wherein the interferent is water and the analytes include at least one non-polar volatile organic compound.6. The method of claim 5 , wherein the at least one non-polar volatile organic compound is benzene or toluene.7. The method of claim 1 , wherein the gas chromatography column has a length claim 1 , an inner diameter and/or a coating thickness selected to enhance complete elution of the interferent before elution of the analyte.8. The method of claim 1 , wherein a length of the gas chromatography column is not greater than about 30 meters.9. The method of claim 1 , wherein an inner diameter of the gas chromatography column is equal to or greater than about 0.53 mm.10. The method of claim 1 , wherein a coating on the gas chromatography column is non-polar and/or has a thickness of at least about 3.0 microns.11. The method of claim 1 , further comprising purging the sample ...

Spin coated stationary phase microfabricated gas chromatographic columns

Presented herein is a new concept of uniformly spin coating a flat surface with a stationary phase and creating a gas chromatography column by pressing a grooved lid, with micro-stamped ridges, down onto the coated substrate. The lids are molded out of commercially available rigid materials including epoxies so that when pressed onto a flat surface it will create an air tight seal. The epoxy material is rendered inert by a thin layer of gold.

Metal matrices for use in high gradient magnetic separation of biological materials and method for coating the same

Improvements in the existing procedures and materials for conduct of high gradient magnetic separation (HGMS) are disclosed. Superior superparamagnetic particles, optionally coated with a polysaccharide or other, usually organic, materials can be prepared in uniform compositions with homogeneous magnetizations. The coating can conveniently be conjugated to a specific binding moiety complementary to a biological material whose purification or separation is desired. In addition, plastic coated matrices which form superior magnetic gradient-intensifying supports are disclosed, along with improved methods and apparatus to conduct HGMS.

Methods for coating metal matrices for use in high gradient magnetic separation of biological materials and method for coating the same

Improvements in the existing procedures and materials for conduct of high gradient magnetic separation (HGMS) are disclosed. Superior superparamagnetic particles, optionally coated with a polysaccharide or other, usually organic, materials can be prepared in uniform compositions with homogeneous magnetizations. The coating can conveniently be conjugated to a specific binding moiety complementary to a biological material whose purification or separation is desired. In addition, plastic coated matrices which form superior magnetic gradient-intensifying supports are disclosed, along with improved methods and apparatus to conduct HGMS.

ガスクロマトグラフ用キヤピラリ−カラム

(57)【要約】本公報は電子出願前の出願データであるた め要約のデータは記録されません。

A method for separating or purifying a biological macromolecule using an improved affinity carrier.

Chromatography technology and equipment

Deactivated capillary columns for use in capillary electrophoresis

The walls of fused-silica capillary columns used for capillary zone electrophoresis and micellar electrokinetic capillary chromatography may be deactivated with polysiloxanes, polysilazanes and other silicone polymers to permit more effective separations without eliminating electro-osmotic flow within the columns.

Gas chromatograph column and its production

(57)【要約】本公報は電子出願前の出願データであるた め要約のデータは記録されません。

Liquid chromatography technique

公开了液相色谱技术。特别地，该液相色谱技术包括提供具有涂覆金属流体接触元件的液相色谱系统，以及输送流体以接触该涂覆金属流体接触元件。流体输送的条件选自由以下组成的组：流体温度大于150℃、驱动流体的压力大于60MPa、流体含有与钛和聚醚醚酮中一种或两种不相容的含蛋白质分析物、流体含有与钛或聚醚醚酮中一种或两种不相容的螯合剂，以及其组合。

Solid phase extraction pipette

Solid phase extraction devices for sample preparation are disclosed, comprising a hollow conical tube having one narrower opening and one broader opening, wherein the narrower opening of the tube contains a solid phase extraction material comprising a functionalized monolithic sorbent, and wherein the solid phase extraction device is prepared by a combination of reduced pressure, positive pressure and mechanical compaction. The solid phase extraction devices are adapted for preparation of small sample volumes, and provide excellent recovery of analytes and good flow characteristics. Methods for preparing and using the solid phase extraction devices are disclosed.

Separation process of biopolymeric molecules and carrier for use in such a process

In the present invention, there is disclosed a separation process of biopolymeric molecules, in particular biopolymeric molecules from the group consisting of mono- and multiphosphorylated peptides, recombinant peptides/proteins with polyhistidine anchor, His-tag, or another chemically similar biologically specific anchor, peptides/proteins containing cysteine and nucleic acids. The process is characterized in that the biopolymeric molecule binds in a binding solution to a carrier, which comprises a core with dimensions in nano- and/or submicro- and/or micro scale, formed by an oxide of at least one transient metal and/or silicon oxide, on the surface of which, there is deposited at least one continuous or discontinuous layer and/or nanoparticles of magnetic metal oxide and/or the nanoparticles are deposited in the internal structure thereof. Subsequently, undesired non-specifically bound component are washed off from the carrier with the bound biomolecules by at least one wash in a washing solution, whereupon biopolymeric molecules are eluted therefrom by the change of pH value or by an eluent solution. The invention also discloses a carrier for use in the above-described process.

Multicapillary device for sample preparation

A multicapillary sample preparation device, especially useful for handling biological samples, comprising a plurality of uniform capillary tubes coated with a stationary phase, and arranged in a monolithic element. The multicapillary device is suitable for attachment to a pipette, micropipette, syringe, or other analytical or sample preparation instrument.

Disposable monolithic column

Permeable polymeric monolithic materials are prepared in a plastic column casing. In one embodiment, the permeable polymeric monolithic materials are polymerized by the application of heat from an external source starting at a low temperature such as 40 degrees centigrade, depending on the mixture and size of the column, and continuing at a higher temperature, such as 60 degrees centigrade. The temperature at the start of the polymerization is low enough so as not to cause exothermal run-away conditions and to avoid high heat of reaction that would prevent a substantially constant temperature across the cross-section of the column. The higher temperature is used after sufficient monomer depletion has occurred and steric interference has increased so the polymerization reaction is sufficiently slow to avoid heat of reaction generation high enough to cause significant reduction in the homogeneousness of the pore sizes.

Solid phase extraction pipette

Solid phase extraction devices for sample preparation are disclosed, comprising a hollow conical tube having one narrower opening and one broader opening, wherein the narrower opening of the tube contains a solid phase extraction material comprising a functionalized monolithic sorbent, and wherein the solid phase extraction device is prepared by a combination of reduced pressure, positive pressure and mechanical compaction. The solid phase extraction devices are adapted for preparation of small sample volumes, and provide excellent recovery of analytes and good flow characteristics. Methods for preparing and using the solid phase extraction devices are disclosed.

Wetting of a plastic bed support for a chromatography column

Chromatographic technique and apparatus

To provide a compact, sensitive comprehensive, two-dimensional gas chromatograph, a chromatographic column has first and second sections in series with each other to permit the flow of sample and a carrier through the first section and the second section. The retention time of the second section is less than the band resolution time of the first section. To control the wave fronts between the first and second sections, first and second heaters are positioned to heat and drive off sample collected at the outlet of the first section for collection in the second section and to heat sample collected at the inlet of the second section so that the first heater rapidly drives off sample for collection in the second section and then the second section rapidly drives off sample in a sharp wave front while the first section is accumulating another band for later movement into the second section.

Method for preparing a monolithic stationary phase, associated method for producing a chromatography column and associated separation method

Deactivated capillary columns for use in electrophoresis and micellar electrokinetic chromatography

Wetting of a plastic bed support for a chromatography column

一种润湿用于色谱柱的塑料床支撑体的方法，其包含以下步骤：提供带有孔结构的塑料床支撑体，所述孔结构中包含空气，并将塑料床支撑体浸泡在包含0.1-30重量%非表面活性剂润湿剂的水性溶液中，导致从所述孔结构去除所述空气的至少约60%。

High efficiency sol-gel gas chromatography column

A capillary column (10) includes a tube structure having inner walls (14) and a sol-gel substrate (16) coated on a portion of inner walls (14) to form a stationary phase coating (18) on inner walls (14). The sol solution used to prepare the sol-gel substrate (16) has at least one baseline stabilizing reagent and at least one surface deactivation reagent resulting in the sol-gel substrate (16) having at least one baseline stabilizing reagent residual and at least one surface deactivating reagent residual. A method of making the sol-gel solution is by mixing suitable sol-gel precursors to form the solution, stablizing the solution by adding at least one baseline stabilization reagent, deactivating the solution by adding at least one surface deactivation reagent to the solution, and reacting the solution in the presence of at least one catalyst.

Separation system, components of a separation system and methods of making and using them

Permeable polymeric monolithic materials are prepared in a column casing. In one embodiment, the permeable polymeric monolithic materials are polymerized while pressure is applied through a piston having a smooth piston head in contact with the polymerization mixture. The pressure eliminates wall effect and changes the structure in the column. Similarly, some columns that have a tendency to swell in the presence of aqueous solutions and pressurized while the solution is applied to prevent swelling and wall effect. This procedure also changes the structure in the column. The size of the separation effective openings can be controlled by the amount of the pressure and pores eliminated. Uniformity in the direction flow is improved by controlling polymerization with radiation rather than with conducted heat.

Method of dynamically applying stationary phase onto capillary column inner surface

Изобретение относитс  к аналитическому приборостроению и может быть использовано в газовой хроматографии дл  получени  капилл рных колонок со слоем неподвижной фазы на их внутренней поверхности. Цель изобретени  - улучшение равномерности сло  неподвижной фазы, сокращение времени его формировани , повышение воспроизводимости способа и увеличение числа примен емых растворителей. Процессы нанесени  сло  неподвижной фазы и удалени  растворител  осуществл ют в термостате, в котором устанавливают и поддерживают температуру, равную температуре кипени  используемого растворител , а окончание формировани  сло  неподвижной фазы определ ют по прекращению образовани  пробок сконденсированных паров растворител  в буферной колонке. 6 ил. 3 (/ The invention relates to analytical instrumentation and can be used in gas chromatography to obtain capillary columns with a stationary phase layer on their inner surface. The purpose of the invention is to improve the uniformity of the stationary phase layer, reduce the time of its formation, increase the reproducibility of the method and increase the number of solvents used. The processes of applying a layer of the stationary phase and removing the solvent are carried out in a thermostat in which the temperature is set equal to the boiling point of the solvent used, and the end of the formation of the layer of the stationary phase is determined by stopping the formation of fused condensate vapors in the buffer column. 6 Il. 3 (/

Procedure for preparing a monolithic stationary phase, procedures for manufacturing a chromatographic column and associated separation

Procedimiento de fabricación de una columna de cromatografía, en particular una columna de cromatografía de separación o de extracción, comprendiendo este procedimiento las siguientes etapas (1) y (2): (1) la preparación de una fase estacionaria monolítica en el volumen interior de la columna de cromatografía, siendo esta columna de cromatografía de polímero termoplástico, realizando las siguientes etapas sucesivas (i) a (iii): (i) la modificación de la pared interna de la columna de cromatografía mediante la realización de las siguientes etapas sucesivas (a) a (c): (a) la preparación de una composición polimerizable de anclaje que comprende: - al menos un monómero de (met)acrilato seleccionado de dimetacrilato de etilenglicol, diacrilato de 1,4-butanodiol, dimetacrilato de trietilenglicol y trimetacrilato de trimetilolpropano, - uno o más disolventes, y - 2,2-dimetoxi-2-fenilacetofenona, (b) el depósito, sobre la pared interna de la columna de cromatografía, de la composición polimerizable de anclaje preparada en la etapa (a), y (c) la polimerización de la composición polimerizable de anclaje mediante irradiación usando rayos ultravioletas; (ii) la introducción de una composición polimerizable de síntesis del monolito en el volumen interior de la columna de cromatografía, comprendiendo la composición polimerizable de síntesis del monolito: - un primer monómero de (met)acrilato seleccionado de dimetacrilato de etilenglicol, diacrilato de 1,4-butanodiol, dimetacrilato de trietilenglicol y trimetacrilato de trimetilolpropano, - un segundo monómero de met(acrilato) seleccionado de metacrilato de alilo, metacrilato de glicidilo, metacrilato de laurilo, metacrilato de butilo, metacrilato de 2-hidroxietilo, di(met)acrilato de polietilenglicol, metacrilato de glicidilo y de bisfenol A y el acrilato de hexilo, - uno o más agentes porógenos y - un iniciador de polimerización por radicales; y (iii) la polimerización de la composición polimerizable de síntesis del monolito y ( ...

Methods to increase sensitivity lc/ms analysis

The present disclosure discusses a method of separating a sample (e.g., pharmaceutical drug, genotoxic impurity, biomarker, and/or biological metabolite) including coating a metallic flow path of a chromatographic system; injecting the sample into the chromatographic system; flowing the sample through the chromatographic system; separating the sample; and analyzing the separated sample using mass spectroscopy. In some examples, the coating applied to the surfaces defining the flow path is non-binding with respect to the sample – and the separated sample. Consequently, the sample does not bind to the low-binding surface of the coating of the flow path. The applied coating can increase the chromatographic peak area for the sample of the chromatographic system.

Separation system, components of a separation system and methods of making and using them

Permeable polymeric monolithic materials are prepared in a column casing. In one embodiment, the permeable polymeric monolithic materials are polymerized while pressure is applied through a piston having a smooth piston head in contact with the polymerization mixture. The pressure eliminates wall effect and changes the structure in the column. Similarly, some columns that have a tendency to swell in the presence of aqueous solutions and pressurized while the solution is applied to prevent swelling and wall effect. This procedure also changes the structure in the column. The size of the separation effective openings can be controlled by the amount of the pressure and pores eliminated.

Coating method of pipe inside

(57)【要約】本公報は電子出願前の出願データであるた め要約のデータは記録されません。

Use of vapor deposition coated flow paths for improved chromatography of metal interacting analytes

A device for separating analytes is disclosed. The device has a sample injector, sample injection needle, sample reservoir container in communication with the sample injector, chromatography column downstream of the sample injector, and fluid conduits connecting the sample injector and the column. The 5 interior surfaces of the fluid conduits, sample injector, sample reservoir container, and column form a flow path having wetted surfaces. A portion of the wetted surfaces of the flow path are coated with an alkylsilyl coating that is inert to at least one of the analytes. The alkylsilyl coating has the Formula I: (I). R1, R2, R3, R4, R5, and R6 are each independently selected from (C1-C6)alkoxy, -NH(C1-C6)alkyl, -N((C1- C6)alkyl)2, OH, ORA, and halo. RA represents a point of attachment to the interior surfaces of the fluidic system. At least one of R1, R2, R3, R4, R5, and R6 is ORA. X is (C1-C20)alkyl, -O[(CH2)2O]1-20-, -(C1- C1 0)[NH(CO)NH(C1-C10)]1- 2 0-, or -(C1-C10)[alkylphenyl(C1-C10)alkyl]1-20-.

Deactivated surfaces for chromatographic separations and methods of making and using the same

Disclosed are deactivated surfaces for use in chromatographic separations, such as capillary gas chromatography, comprising a surface material coated with a deactivating polymer comprising high surface energy-generating groups and groups for end-capping reactive silanols. Also disclosed are columns comprising such surfaces, methods of making and using the surfaces, and kits for facilitating the same.

Suppression of electroosmosis with hydrolytically stable coatings

STRUCTURAL SURFACES MODIFIED WITH BIDENTATE SILANES.

Separation system, components of a separation system and methods of making and using them

Permeable polymeric monolithic materials are prepared in a column casing. In one embodiment, the permeable polymeric monolithic materials are polymerized while pressure is applied through a piston having a smooth piston head in contact with the polymerization mixture. The pressure eliminates wall effect and changes the structure in the column. Similarly, some columns that have a tendency to swell in the presence of aqueous solutions and pressurized while the solution is applied to prevent swelling and wall effect. This procedure also changes the structure in the column. The size of the separation effective openings can be controlled by the amount of the pressure and pores eliminated. Uniformity in the direction flow is improved by controlling polymerization with radiation rather than with conducted heat.

Devices having an inert surface and methods of making same

Method for covalently attaching polymeric monoliths to polyether ether ketone (PEEK) surfaces

The present invention provides a method of covalently attaching a polymeric monolith to the internal surface of polyether ether ketone (PEEK) tubing and column housings, comprising the steps of: (a) reducing the ketone group of the PEEK to a hydroxyl group to obtain a modified PEEK, (b) optionally reacting the hydroxyl group obtained in step (a) with a compound having an active vinyl group to form a modified PEEK selected from the group of acrylate modified PEEK, methacrylate modified PEEK, styrene modified PEEK and epoxy modified PEEK, and (c) reacting the modified PEEK obtained in step (a) or (b) with a polymer or polymerization mixture for forming the polymeric monolith. Hereby, the mechanical stability and solvent durability of larger diameter monolithic columns as well as their overall performance are improved.

Metal components with inert vapor phase coating on internal surfaces

Patent Application Atty Docket No. 20120138-02 Abstract The invention provides metal liquid chromatography components with uniformly coated internal surfaces and methods for achieving the same. The invention addresses the problem of corrosion or interference of metal components in the flow path for LC analyses in which the sample interacts with metal ions or surfaces. The invention also alleviates the difficulties in coating very long metal tubes and very small metal channels with an inert, continuous coating that adheres well to metal surfaces. The metal flow path is rendered inert by the coating, and thus compatible with bioanalytical separations, for example, by using a vapor phase deposition process to coat the inner surfaces with a coating that continuously covers all metal surfaces in the flow path. Patent Application Atty Docket No. 20120138-02 FIG. 1. Schematic illustration of an exemplary embodiment of the invention with dual layers of coatings

Method of making ionic liquid mediated sol-gel sorbents

Ionic liquid (IL)-mediated sol-gel hybrid organic-inorganic materials present enormous potential for effective use in analytical microextraction. One obstacle to materializing this prospect arises from high viscosity of ILs significantly slowing down sol-gel reactions. A method was developed which provides phosphonium-based, pyridinium-based, and imidazolium-based IL-mediated advanced sol-gel organic-inorganic hybrid materials for capillary microextraction. Scanning electron microscopy results demonstrate that ILs can serve as porogenic agents in sol-gel reactions. IL-mediated sol-gel coatings prepared with silanol-terminated polymers provided up to 28 times higher extractions compared to analogous sol-gel coatings prepared without any IL in the sol solution. This study shows that IL-generated porous morphology alone is not enough to provide effective extraction media: careful choice of the organic polymer and the precursor with close sol-gel reactivity must be made to ensure effective chemical bonding of the organic polymer to the created sol-gel material to be able to provide the desired sorbent characteristics.

Chromatography method

Method for exchanging materials, wherein a gaseous, liquid or supercritical mobile phase containing species to be separated is circulated through a packing comprising a stationary phase, the method being characterised in that: - the packing comprises a plurality of capillary ducts formed in at least one first material, the ducts passing through the packing between an upstream face through which the mobile phase enters the packing and a downstream face through which the mobile phase leaves the packing, - each duct comprises, on at least one portion of the inner wall thereof, at least one secondary material consisting of an organic gel or porous mineral, - the thickness of the secondary material defines, inside the duct, at least one empty tubular channel of solid material, the channel being open so as to allow the mobile phase to enter and extending continuously between the upstream and downstream faces of the capillary duct - the secondary material has a thickness between 0.05 times and 0.5 times the diameter of the channel - the method is carried out with a velocity of the mobile phase between 5.0 times and 50 times the speed of the optimum mobile phase defined by the minimum of the Van Deemter curve of the majority separating compound under the method conditions - the cumulative volume of the capillary ducts is more than 15% of the total packing volume.

Method for the preparation of monolithic columns

制备分离柱或在微制装置中的通道的方法，包括以下步骤：提供未填充的柱或在微制装置中的通道；用活化剂活化柱或通道的内壁；用包含单体、至少一种成孔剂和至少一种聚合引发剂的混合物的聚合溶液填充柱；和在柱或通道中聚合所述混合物以形成刚性多孔整料聚合物塞。所述方法特征在于所述单体包含作为主要单体的二乙烯基苯和丙烯酸异癸酯的混合物，和所述至少一种成孔剂包含异丁醇。

Gas chromatograph column with carbon nanotube-bearing channel

A carbon nanostructured micro-fabricated gas chromatography column which is particularly well-suited to the surface well-site and/or the downhole analysis of natural gas in oilfield or gasfield applications (but which may also be used in non-oilfield or non-gasfield situations) is described. This micro-fabricated column integrates a micro-structured substrate such as a silicon substrate with carbon nanotubes as an active nanostructured material in a micro-channel. Benefits of the present invention include enhanced separation of alkanes and isomers, particularly below hexane (i.e., below C 6 ), as well as the separation of carbon dioxide, hydrogen sulfide, and water and other substances present in natural gas. The chromatography column of the present invention is in one embodiment a part of an entire gas chromatograph system that in its simplest form also comprises an injector and a detector. Preferably the injector, separation column, and detector are all micro-fabricated on a substrate.

Multi column chromatography system

Devices Having An Inert Surface And Methods Of Making Same

The present invention features devices and methods of making such devices for performing liquid chromatography having at least one wetted surface having a composition of a polysilazane.

Solid phase extraction device

Festphasen-Extraktionsvorrichtung für die Probenherstellung umfassend ein hohles, konisches Rohr mit einer engeren Öffnung und einer breiteren Öffnung, wobei die engere Öffnung des Rohres ein Festphasen-Extraktionsmaterial, das ein funktionalisiertes, monolithisches Sorptionsmittel umfasst, enthält, dadurch gekennzeichnet, dass die Festphasen-Extraktionsvorrichtung durch eine Kombination von bezogen auf Atmosphärendruck reduziertem Druck, bezogen auf Atmosphärendruck erhöhtem Druck und mechanischer Verdichtung hergestellt ist, und wobei das funktionalisierte, monolithische Sorptionsmittel eine Glasfasermatrix, die eine Verbundphase aus einem Metall- oder Halbmetalloxid enthält, umfasst. A solid phase extraction apparatus for sample preparation comprising a hollow conical tube having a narrower opening and a wider opening, the narrower opening of the tube containing a solid phase extraction material comprising a functionalized monolithic sorbent, characterized in that the solid phase extraction device is prepared by a combination of reduced pressure relative to atmospheric pressure, increased pressure and mechanical compaction, and wherein the functionalized monolithic sorbent comprises a glass fiber matrix containing a composite phase of a metal or semimetal oxide.

Low pollutant dialysis solution

Use of vapor deposition coated flow paths for improved chromatography of metal interacting analytes

A device for separating analytes is disclosed. The device has a sample injector, sample injection needle, sample reservoir container in communication with the sample injector, chromatography column downstream of the sample injector, and fluid conduits connecting the sample injector and the column. The 5 interior surfaces of the fluid conduits, sample injector, sample reservoir container, and column form a flow path having wetted surfaces. A portion of the wetted surfaces of the flow path are coated with an alkylsilyl coating that is inert to at least one of the analytes. The alkylsilyl coating has the Formula I: (I). R1, R2, R3, R4, R5, and R6 are each independently selected from (C1-C6)alkoxy, -NH(C1-C6)alkyl, -N((C1- C6)alkyl)2, OH, ORA, and halo. RA represents a point of attachment to the interior surfaces of the fluidic system. At least one of R1, R2, R3, R4, R5, and R6 is ORA. X is (C1-C20)alkyl, -O[(CH2)2O]1-20-, -(C1- C1 0)[NH(CO)NH(C1-C10)]1- 2 0-, or -(C1-C10)[alkylphenyl(C1-C10)alkyl]1-20-.

Disposable monolithic column

Permeable polymeric monolithic materials are prepared in a plastic column casing. In one embodiment, the permeable polymeric monolithic materials are polymerized by the application of heat from an external source starting at a low temperature such as 40 degrees centigrade, depending on the mixture and size of the column, and continuing at a higher temperature, such as 60 degrees centigrade. The temperature at the start of the polymerization is low enough so as not to cause exothermal run-away conditions and to avoid high heat of reaction that would prevent a substantially constant temperature across the cross-section of the column. The higher temperature is used after sufficient monomer depletion has occurred and steric interference has increased so the polymerization reaction is sufficiently slow to avoid heat of reaction generation high enough to cause significant reduction in the homogeneousness of the pore sizes.

Liquid chromatography technique

Liquid chromatography techniques are disclosed. Specifically, the liquid chromatography technique includes providing a liquid chromatography system having a coated stainless steel fluid contacting element; and transporting a fluid to contact the coated stainless-steel fluid-contacting element; wherein the fluid includes adenosine triphosphate; wherein the coated stainless steel fluid-contacting element has a coating, the coating including carbon, silicon, oxygen, and hydrogen.

Liquid chromatography technique

Liquid chromatography techniques are disclosed. Specifically, the liquid chromatography technique includes providing a liquid chromatography system having a coated stainless steel fluid contacting element; and transporting a fluid to contact the coated stainless-steel fluid-contacting element; wherein the fluid includes adenosine triphosphate; wherein the coated stainless steel fluid-contacting element has a coating, the coating including carbon, silicon, oxygen, and hydrogen.

反応容器内表面のコーティング方法

Spin coated stationary phase microfabricated gas chromatographic columns

Presented herein is a new concept of uniformly spin coating a flat surface with a stationary phase and creating a gas chromatography column by pressing a grooved lid, with micro-stamped ridges, down onto the coated substrate. The lids are molded out of commercially available rigid materials including epoxies so that when pressed onto a flat surface it will create an air tight seal. The epoxy material is rendered inert by a thin layer of gold.

Spin coated stationary phase microfabricated gas chromatographic columns

Presented herein is a new concept of uniformly spin coating a flat surface with a stationary phase and creating a gas chromatography column by pressing a grooved lid, with micro-stamped ridges, down onto the coated substrate. The lids are molded out of commercially available rigid materials including epoxies so that when pressed onto a flat surface it will create an air tight seal. The epoxy material is rendered inert by a thin layer of gold.

Repressione di elettroosmosi con rivestimenti idroliticamente stabili

Microcrystalline cellulose particle supported sol-gel sorbents

Solid phase extraction (SPE) sorbents and liquid chromatography (LC) stationary phases are provided, as well as methods of fabricating the same. The SPE sorbents and LC stationary phases can use microcrystalline cellulose particles as the substrate and sol-gel sorbent coating technology as the polymer/sorbent immobilization technology. The SPE sorbents and LC stationary phases are stable in a pH range of 1-13 and at a temperature of up to 350 ° C.

Liquid chromatography technique

液体クロマトグラフィー技術

【課題】迅速、小型、高精度、費用効率の良いＬＣ技術を提供する。【解決手段】ＬＣ技術は、被覆金属流体接触エレメントを備える液体クロマトグラフィーシステムを用意するステップと、流体を輸送して被覆金属流体接触エレメントに接触させるステップとを含む。流体を輸送するステップの条件は、流体の温度が摂氏１５０度よりも高いこと、流体を推進する圧力が６０ＭＰａよりも高いこと、流体が、チタンおよびポリエーテルエーテルケトンの一方と不相溶性のタンパク質含有分析物を有すること、流体が、チタンまたはポリエーテルエーテルケトンの一方または両方と不相溶性のキレート化剤を有することからなる群から選択される。【選択図】図２

液体クロマトグラフィー技術

用于肽图分析的低结合表面

本公开论述了一种分离样品(例如，肽化合物)的方法，该方法包括涂覆色谱系统的流动路径；将样品注入到色谱系统中；使样品流动通过色谱系统；分离样品；以及分析分离的样品。在一些示例中，施加到限定流动路径的表面的涂层相对于样品以及分离的样品是非结合性的。因此，样品不与流动路径的涂层(例如，有机二氧化硅涂层)的低结合表面结合。所施加的涂层可减少色谱系统的样品的峰拖尾以及增加分析物回收率。

Liquid chromatography based detection and quantitation of phospho prodrugs and their active metabolites

The present disclosure relates to the use of vapor deposition coated flow paths for improved chromatography and sample analysis using liquid chromatography – mass spectrometry (LC/MS) or liquid chromatography –optical detection (LC/UV). More specifically, this technology relates to separating and quantitation of analytes (e.g., phospho prodrugs and its phosphorylated metabolites) from a sample matrix (e.g., mammalian blood, plasma) using chromatographic devices and fluidic systems having coated flow paths. The LC-MS or LC-UV techniques provide improved recovery, peak shape and dynamic range in the analysis of the prodrug and its metabolites.

Use of vapor deposition coated flow paths for improved chromatography of metal interacting analytes

A device for separating analytes is disclosed. The device has a sample injector, sample injection needle, sample reservoir container in communication with the sample injector, chromatography column downstream of the sample injector, and fluid conduits connecting the sample injector and the column. The interior surfaces of the fluid conduits, sample injector, sample reservoir container, and column form a flow path having wetted surfaces. A portion of the wetted surfaces of the flow path are coated with an alkylsilyl coating that is inert to at least one of the analytes. The alkylsilyl coating has the Formula I: R 1 , R 2 , R 3 , R 4 , R 5 , and R 6 are each independently selected from (C 1 -C 6 )alkoxy, —NH(C 1 -C 6 )alkyl, —N((C 1 -C 6 )alkyl) 2 , OH, OR A , and halo. R A represents a point of attachment to the interior surfaces of the fluidic system. At least one of R 1 , R 2 , R 3 , R 4 , R 5 , and R 6 is OR A . X is (C 1 -C 20 )alkyl, —O[(CH 2 ) 2 O] 1-20 , -(C 1 -C 10 )[NH(CO)NH(C 1 -C 10 )] 1-20 -, or -(C 1 -C 10 )[alkylphenyl(C 1 -C 10 )alkyl] 1-20 -.

气相沉积涂覆的流动路径用于改善金属相互作用分析物的色谱法的用途

本发明公开了一种用于分离分析物的装置。所述装置具有样品注射器，样品注射针，与所述样品注射器连通的样品贮存器容器，在所述样品注射器下游的色谱柱，以及连接所述样品注射器和所述柱的流体导管。所述流体导管、所述样品注射器、所述样品贮存器容器和所述柱的5个内表面形成具有润湿表面的流动路径。所述流动路径的所述润湿表面的一部分涂覆有烷基甲硅烷基涂层，所述烷基甲硅烷基涂层对所述分析物中的至少一种是惰性的。所述烷基甲硅烷基涂层具有式I： R 1 、R 2 、R 3 、R 4 、R 5 和R 6 各自独立地选自(C 1 ‑C 6 )烷氧基、‑NH(C 1 ‑C 6 )烷基、‑N((C 1 ‑C 6 )烷基) 2 、OH、OR A 和卤。R A 表示与流体系统的内表面的连接点。R 1 、R 2 、R 3 、R 4 、R 5 和R 6 中的至少一个为OR A 。X为(C 1 ‑C 20 )烷基、‑O[(CH 2 ) 2 O] 1‑20 ‑、‑(C 1 ‑C 10 )[NH(CO)NH(C 1 ‑C 10 )] 1‑20 ‑或‑(C 1 ‑C 10 )[烷基苯基(C 1 ‑C 10 )烷基] 1‑20 ‑。

气相沉积涂覆的流动路径用于改善金属相互作用分析物的色谱法的用途

本发明公开了一种用于分离分析物的装置。所述装置具有样品注射器，样品注射针，与所述样品注射器连通的样品贮存器容器，在所述样品注射器下游的色谱柱，以及连接所述样品注射器和所述柱的流体导管。所述流体导管、所述样品注射器、所述样品贮存器容器和所述柱的5个内表面形成具有润湿表面的流动路径。所述流动路径的所述润湿表面的一部分涂覆有烷基甲硅烷基涂层，所述烷基甲硅烷基涂层对所述分析物中的至少一种是惰性的。所述烷基甲硅烷基涂层具有式I： R 1 、R 2 、R 3 、R 4 、R 5 和R 6 各自独立地选自(C 1 ‑C 6 )烷氧基、‑NH(C 1 ‑C 6 )烷基、‑N((C 1 ‑C 6 )烷基) 2 、OH、OR A 和卤。R A 表示与流体系统的内表面的连接点。R 1 、R 2 、R 3 、R 4 、R 5 和R 6 中的至少一个为OR A 。X为(C 1 ‑C 20 )烷基、‑O[(CH 2 ) 2 O] 1‑20 ‑、‑(C 1 ‑C 10 )[NH(CO)NH(C 1 ‑C 10 )] 1‑20 ‑或‑(C 1 ‑C 10 )[烷基苯基(C 1 ‑C 10 )烷基] 1‑20 ‑。

Use of vapor deposition coated flow paths for improved chromatography of metal interacting analytes

Use of vapor deposition coated flow paths for improved analytical analysis

A device for processing samples is disclosed. Interior surfaces of the device, which come in contact with fluids, define wetted surfaces. A portion of the wetted surfaces are coated with an alkylsilyl coating having the Formula I: R 1 , R 2 , R 3 , R 4 , R 5 , and R 6 are each independently selected from (C 1 -C 6 )alkoxy, —NH(C 1 -C 6 )alkyl, —N((C 1 -C 6 )alkyl) 2 , OH, OR A , and halo. R A represents a point of attachment to the interior surfaces of the fluidic system. At least one of R 1 , R 2 , R 3 , R 4 , R 5 , and R 6 is OR A . X is (C 1 -C 20 )alkyl, —O[(CH 2 ) 2 O] 1-20 -, —(C 1 -C 10 )[NH(CO)NH(C 1 -C 10 )] 1-20 -, or —(C 1 -C 10 )[alkylphenyl(C 1 -C 10 )alkyl] 1-20 -.

Lc/ms adduct mitigation by vapor deposition coated surfaces

The present disclosure discusses a method of separating a sample (e.g., small organic acid metabolite) including coating a flow path of a chromatographic system. The coating along the flow path is vapor deposited and prevents or severely decreases metal interactions between the metallic chromatographic system and the sample.

Liquid chromatography technique

用于色谱效应的经涂覆的流动路径部件

本公开涉及使用色谱法确定样品中的分析物。本公开提供了从样品中分离分析物的方法。该方法包括将包含该分析物的样品引入色谱系统中。该色谱系统具有：设置在该色谱系统内部的流动路径，该流动路径的至少一部分具有活性涂层；以及在该色谱柱内部具有固定相材料的色谱柱，该固定相材料有利于通过与该样品中的至少一种分析物相互作用来分离该样品中的该分析物。将该活性涂层选择成通过(1)排斥力、(2)次级相互作用或(3)与该固定相材料相互作用不同的保留机制与该样品中的至少一种分析物相互作用。

Use of vapor deposition coated flow paths for improved chromatography of metal interacting analytes

A device for separating analytes is disclosed. The device has a sample injector, sample injection needle, sample reservoir container in communication with the sample injector, chromatography column downstream of the sample injector, and fluid conduits connecting the sample injector and the column. The interior surfaces of the fluid conduits, sample injector, sample reservoir container, and column form a flow path having wetted surfaces. A portion of the wetted surfaces of the flow path are coated with an alkylsilyl coating that is inert to at least one of the analytes. The alkylsilyl coating has the Formula I:R¹, R², R³, R⁴, R⁵, and R⁶ are each independently selected from (C₁-C₆)alkoxy, -NH(C₁-C₆)alkyl, -N((C₁-C₆)alkyl)₂, OH, OR^A, and halo. R^A represents a point of attachment to the interior surfaces of the fluidic system. At least one of R¹, R², R³, R⁴, R⁵, and R⁶ is OR^A. X is (C₁-C₂₀)alkyl, -O[(CH₂)₂O]_1-20-, -(C₁-C₁₀)[NH(CO)NH(C₁-C₁₀)]_1-20-, or -(C₁-C₁₀)[alkylphenyl(C₁-C₁₀)alkyl]_1-20-.

Methods to increase sensitivity of LC/MS analysis

The present disclosure discusses a method of separating a sample (e.g., pharmaceutical drug, genotoxic impurity, biomarker, and/or biological metabolite) including coating a metallic flow path of a chromatographic system; injecting the sample into the chromatographic system; flowing the sample through the chromatographic system; separating the sample; and analyzing the separated sample using mass spectroscopy. In some examples, the coating applied to the surfaces defining the flow path is non-binding with respect to the sample—and the separated sample. Consequently, the sample does not bind to the low-binding surface of the coating of the flow path. The applied coating can increase the chromatographic peak area for the sample of the chromatographic system.

一种毛细管色谱柱涂覆装置

本发明的目的在于提供一种毛细管色谱柱涂覆装置，包括:密封容器和压力单元；密封容器的容器壁上分别设置有色谱柱连接孔、进气口和可开闭的密封门，密封容器的内腔还设置有固定架；在使用状态下，盛放涂覆液的容器通过密封门进入密封容器的内腔，并置于固定架上，密封容器和压力单元通过进气口连通。现有技术中主要的涂覆装置仅由加压装置和单个的密封容器构成，密封容器内的空间仅可以放一个试管，密封容器顶部设置有大螺帽，在大螺帽上再设置一小的色谱柱连接孔用于插入和固定毛细管色谱柱，这样的毛细管色谱柱涂覆装置存在操作难度大、操作不方便、危险高和生产效率低的问题。

一种毛细管色谱柱涂覆装置

本发明的目的在于提供一种毛细管色谱柱涂覆装置，包括:密封容器和压力单元；密封容器的容器壁上分别设置有色谱柱连接孔、进气口和可开闭的密封门，密封容器的内腔还设置有固定架；在使用状态下，盛放涂覆液的容器通过密封门进入密封容器的内腔，并置于固定架上，密封容器和压力单元通过进气口连通。现有技术中主要的涂覆装置仅由加压装置和单个的密封容器构成，密封容器内的空间仅可以放一个试管，密封容器顶部设置有大螺帽，在大螺帽上再设置一小的色谱柱连接孔用于插入和固定毛细管色谱柱，这样的毛细管色谱柱涂覆装置存在操作难度大、操作不方便、危险高和生产效率低的问题。

カラム

(57)【要約】本公報は電子出願前の出願データであるた め要約のデータは記録されません。

Liquid chromatography technique

LC techniques are disclosed. The LC technique includes providing a liquid chromatography system having a coated metallic fluid-contacting element, and transporting a fluid to contact the coated metallic fluid contacting element. Conditions for the transporting of the fluid are selected from the group consisting of the temperature of the fluid being greater than 150 degree Celsius, pressure urging the fluid being greater than 60 MPa, the fluid having a protein-containing analyte incompatible with one of titanium and polyether ether ketone, the fluid having a chelating agent incompatible with the one or both of the titanium or the polyether ether ketone.

Method for coating the internal surface of a reaction vessel

A method for coating the internal surfaces of a reaction vessel having a small internal diameter comprises the steps of (i) introducing into the reaction vessel a solution of one or more monomers in a suitable solvent; (ii) introducing a flow of an inert gas through the reaction vessel; and (iii) initiating polymerization of the monomer solution.