Preparation method of fenugreek oil in fenugreek, macromolecular fractions such as vegetable proteins and micromolecular fractions such as dioscin

Technical Field

The invention relates to a method for extracting of raw materials for pharmaceuticals, in particular to a semen Trigonellae in semen Trigonellae oil, vegetable protein, and other large molecules, and clusters of walnut dioscin method for the preparation of small molecules.

Technical background

Fenugreek seed by seed, and cotyledons a endosperm, wherein spermoderm account for the weight of the seeds 10%-15%, of the weight of the seed endosperm accounted for 35%-40%, cotyledons total seed weight of 45%-55%. Semen Trigonellae cotyledons is rich in semen Trigonellae oil, protein and saponin, flavone, alkloids, small molecule parts such as non-protein non-acid group.

Semen Trigonellae oil mainly containing unsaturated fatty acid, fatty acid total for 78.91%, wherein the linoleic acid and linolenic acid content is very high, are respectively occupied 43.60% and 34.72%, and for the same 78.32%. Unsaturated fatty acid with reduced triglyceride in blood fat and anti-oxidation, anti-free radical, anti-tumor, enhance immune function, the higher the content of the same to prevent the formation of thrombus. Linoleic acid is similar to the role of vitamin E, can play the role of preventing atherosclerosis. Linoleic acid is essential fatty acids, cannot synthesize in the human body, can only from food intake. Therefore the development of semen Trigonellae seed oil of important significance.

Semen Trigonellae in the content of plant protein is 16.97%, it is a kind of green, security health food, also can be used as a high-grade animal feed. If only as a single plant protein treatment, there is no economic benefit, but through the integrated use of extracting semen Trigonellae protein, can reduce the cost, increase the economic benefits.

Micromolecule part group different characteristics because of its structure, thus presents different biological activity and pharmacological efficacy, can be used as an important medical industrial raw materials.

Currently, semen Trigonellae oil, walnut, and small-molecule protein preparation with two process line, method a:to semen Trigonellae seeds as the raw material, by a crushing, extracting, separating the first oil and semen Trigonellae hu Luba powder , after through leaching hu Luba powder , protein teherated, walnut, separation micromolecule sequentially, alcohol sink final glue, dried semen Trigonellae glue.

The shortcoming of the method a:

1. In order to of fenugreek seeds as the raw material, without first removing the endosperm part, lead to large viscosity extract, extract for the follow-up effective substance difficult.

2. Proteins are as waste, has not been effectively utilized.

3. Final separation tonka bean rubber , impact on the quality of the, no economic advantage.

Method two: to semen Trigonellae after the de-gumming the remaining portion of the raw material, the crushing, extraction, preparation hu Luba oil , after acid hydrolysis the filtered residue as walnut, extracting small molecules, the remaining elements are used as animal feed.

The disadvantages of the second method:

1. To the remaining portion of the raw material after the degumming, because the mixed with the endosperm part, the extraction system to high viscosity, apt to agglomerate, to the development of the downstream products of difficulties.

2. Semen Trigonellae oil and protein transfer rate is low and has not been effectively utilized.

3. Direct hydrolysis of protein damage, the remaining elements are used as animal feed, very poor taste, are not comprehensive utilization, but also the water consumption is large, the pressure of the environment.

Content of the invention

The purpose of this invention is to solve the disadvantages of the above-mentioned technical background, semen Trigonellae in providing a semen Trigonellae oil, vegetable protein, and other large molecules, and clusters of walnut dioscin method for the preparation of small molecules.

To achieve the above object, this invention adopts the following technical solutions: a semen Trigonellae in semen Trigonellae oil, vegetable protein, and other large molecules, and clusters of walnut dioscin method for the preparation of small molecules, the preparation method comprises the following steps:

A. Preparation of hu Luba oil : to semen Trigonellae cotyledons as raw materials, by crushing, screening, extraction and separation, to obtain defatted seed leaf powder and semen Trigonellae oil;

B. Plant protein preparation of large molecules such as walnut, :

(1) step a dispersed in the solvent in degreasing seed leaf powder , grinding in a grinding machine, by the separation to obtain filtrate and seed leaf dregs ;

(2) step (1) the resulting filtrate is separated by the multi-stage membrane filtration system, and the obtained liquid;

(3) step (2) the resulting retention solution is concentrated, drying plant protein, and other large molecular sites group.

C. Preparation of small molecule of walnut, : the step (2) the too liquid is concentrated, group shall be small molecule part.

In said step a, the semen Trigonellae cotyledons the requirement of raw materials: spermoderm content <5%, the content of the endosperm of <5%, the moisture content <8%.

The steps of the method for extracting a: supercritical extraction, organic solvent extraction, steam distillation, expression of one or a combination of several kinds.

Wherein, when the supercritical extraction, extraction pressure is 20-50MPa, extraction temperature the 20-60 [...] , the extraction time 0.5-4h, the extraction flow rate is 8-60L/h, cosolvent is ethanol, methanol, butanol, acetone, ethyl acetate or a mixture of several of, the feed liquid than (g/mL) the 1 [...] 0.1-1 the [...] 3. When using the organic solvent extraction, the used organic solvent is ethanol, petroleum ether, cyclohexane, hexane, gasoline, 1, 2-dimethoxy ethane one kind or in a combination of several kinds.

The steps in a method for the separation of the centrifugal separation, the rotational speed is 3000-6000r/min, time 30-90min.

In said step b, the solvent is 20%-90% ethanol, butanol, isobutanol or of a combination of some kind.

In said step b the grinding time is 1-6h, the rotational speed is 800-2000r/min; separating the way to the centrifugal, press filtration, vacuum filtration, in natural sedimentation of one kind or a few kinds of mixing.

Said step b to a membrane filtration system multistage ceramic film, 10 million molecular weight film and 1 million molecular weight film combination.

In said step b the obtained concentrated manner perconcentration, in multi-stage flash evaporation concentration of one or a combination of several kinds.

Obtained in said step b the drying is vacuum drying, freeze drying, spray drying, microwave drying and infrared drying in one or some of the combination of several kinds.

In the step c, the liquid concentration of the concentrated way to multi-stage flash distillation, multi-effect vacuum concentration.

In the step c, the liquid film drying way to freeze drying, spray drying, microwave drying and infrared drying in one or some of the combination of several kinds.

Compared with the prior art, has the beneficial effects of this invention are as follows:

1. To semen Trigonellae cotyledons as raw material for preparing semen Trigonellae oil, vegetable protein macromolecule such as the small molecule group and neuropsychosis position, compared with the more traditional method, the cotyledons in the endosperm of cohesiveness, caking phenomena, reduces the difficulties of green technology development downstream, improves the purity of the product.

2. Trituration with with the organic solvent, the extraction temperature is low, reducing the protein large group of small molecule of walnut, and extent destroying the structure, reduce the dissolution of the impurity.

3. Semen Trigonellae oil, vegetable protein macromolecule such as the preferential separation of clusters, the degree of enrichment of the downstream products is improved, reducing the separation pressure, so as to be fully comprehensive utilization of fenugreek seeds.

4. Small molecule part dioscin high enrichment because group nature significant difference is difficult to be separated, can be used as the raw materials of pharmaceutical industry.

Description of drawings

Figure 1 is the production flow chart of the invention a semen Trigonellae glue;

Mode of execution

The purpose of the present invention in order to more clearly understand and advantages, the following binding embodiment of further details of the invention. It should be understood, the specific embodiment described in order to explain the invention only, is not used to limit the invention.

As shown in Figure 1. The invention a semen Trigonellae in semen Trigonellae oil, vegetable protein, and other large molecules, and clusters of walnut dioscin method for the preparation of small molecules, characterized in that the preparation method comprises the following steps:

A. Preparation of hu Luba oil : to semen Trigonellae cotyledons as raw materials, by crushing, screening, extraction and separation, to obtain defatted seed leaf powder and semen Trigonellae oil;

B. Plant protein preparation of large molecules such as walnut, :

(1) step a dispersed in the solvent in degreasing seed leaf powder , grinding in a grinding machine, by the separation to obtain filtrate and seed leaf dregs ;

(2) step (1) the resulting filtrate is separated by the multi-stage membrane filtration system, and the obtained liquid;

(3) step (2) the resulting retention solution is concentrated, drying plant protein, and other large molecular sites group.

C. Preparation of small molecule of walnut, : the step (2) the too liquid is concentrated, group shall be small molecule part.

Example a

The semen Trigonellae cotyledons 0.5 kg, selected, spermoderm content <5%, the content of the endosperm of <5%, the moisture content <8%, crushing and screening, the supercritical extraction tank, extracting 2h, the temperature of the 40 [...] , flow rate is 25L/h, the pressure 35 MPa, are respectively oil is collected and degreasing seed leaf powder , grease part, by vacuum distillation to obtain semen Trigonellae oil 52.07g, the yield is about 10.41%. seed leaf powdertakes the degreasing , in 40% ethanol to grind 2h, speed 1200r/min, suspension natural sedimentation 4h, reclosable pouring supernatant fluid, passes through the ceramic, 10 million molecular weight film and 1 million molecular weight membrane filtration system, through the multi-stage flash evaporation concentrate obtained, such as freeze drying plant protein group of large molecular part 61g, the extraction rate is 12.2%. The liquid film through the multi-effect vacuum concentrated, spray drying to obtain the small molecule sites group 142.2g, the extraction rate is 28.44%.

Example II

The semen Trigonellae cotyledons 1 kg, selected, spermoderm content <5%, the content of the endosperm of <5%, the moisture content <8%, crushing and screening, the 10L extraction pot, respectively for 5L petroleum extracted 3 times, the temperature of the 75 [...] , each 2h, suspension centrifugal, speed 3000r/min, time 30 min, collecting ether fluid and degreasing seed leaf powder respectively, by the reduced pressure distillation to ether fluid semen Trigonellae oil 112.2g, the extraction rate is 11.22%. seed leaf powdertakes the degreasing , in 60% ethanol to grind 4h, speed 1000r/min, suspension fluid filter pressing , heating liquid passes through the ceramic, 10 million molecular weight film and 1 million molecular weight membrane filtration system, through the multi-stage flash evaporation obtained concentrated, dried under vacuum to get the plant protein macromolecule part group and 119g, the extraction rate is 11.9%. The liquid spray drying to obtain the small molecule sites group 272.4g, the extraction rate is 27.24%.

Example three

The semen Trigonellae cotyledons 1 kg, selected, spermoderm content <5%, the content of the endosperm of <5%, the moisture content <8%, crushing and sieving, in the continuous extraction tank, cyclonexane continuous extraction 6h, temperature of the 85 [...] , degreasing and respectively collect seed leaf powder cyclohexane, cyclohexane solution by reduced pressure distillation shall be semen Trigonellae oil 11.98g, the extraction rate is 11.98%. seed leaf powdertakes the degreasing , in the n-butanol grinds 6h, speed 900r/min, suspension centrifugal, speed 6000r/min, time 30 min, the supernatant fluid once, passes through the ceramic, 10 million molecular weight film and 1 million molecular weight membrane filtration system, spray drying plant protein obtained large molecular part group such as 117.8g, the extraction rate is 11.78%. The concentration-effect vacuum the membrane fluid are many , microwave drying to obtain the small molecule sites group 280.9g, the extraction rate is 28.09%.

Table 1

As shown in table 1 illustrated, the conversion rate of the present invention is significantly higher than that of the method a second method.

The stated above is the preferred embodiment of the invention, it should be noted that, in the technical field as the ordinary technical personnel, without breaking away from the premise of the principle of the present invention, can also be made a number of improvements and retouches, these improvements and retouches should also be regarded as the scope of protection of this invention.