CN1456570A - Extraction of saponin from seeds of trigonella foenum-graecum - Google Patents
Extraction of saponin from seeds of trigonella foenum-graecum Download PDFInfo
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- CN1456570A CN1456570A CN 03118627 CN03118627A CN1456570A CN 1456570 A CN1456570 A CN 1456570A CN 03118627 CN03118627 CN 03118627 CN 03118627 A CN03118627 A CN 03118627A CN 1456570 A CN1456570 A CN 1456570A
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- Prior art keywords
- saponin
- fenugreek seed
- extracting
- actives
- extraction
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- 239000001397 quillaja saponaria molina bark Substances 0.000 title claims abstract description 32
- 229930182490 saponin Natural products 0.000 title claims abstract description 32
- 150000007949 saponins Chemical class 0.000 title claims abstract description 31
- 238000000605 extraction Methods 0.000 title claims description 12
- 244000250129 Trigonella foenum graecum Species 0.000 title 1
- 235000001484 Trigonella foenum graecum Nutrition 0.000 title 1
- 235000001019 trigonella foenum-graecum Nutrition 0.000 title 1
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000007864 aqueous solution Substances 0.000 claims abstract description 9
- 108010059892 Cellulase Proteins 0.000 claims abstract description 6
- 229940106157 cellulase Drugs 0.000 claims abstract description 6
- 239000011347 resin Substances 0.000 claims abstract description 6
- 229920005989 resin Polymers 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 101710173866 Seminase Proteins 0.000 claims abstract description 4
- 239000001917 trigonella foenum graecum l. absolute Substances 0.000 claims description 15
- 210000000582 semen Anatomy 0.000 claims description 10
- 238000005238 degreasing Methods 0.000 claims description 9
- 239000000284 extract Substances 0.000 claims description 7
- 108090000790 Enzymes Proteins 0.000 claims description 6
- 102000004190 Enzymes Human genes 0.000 claims description 6
- 229940088598 enzyme Drugs 0.000 claims description 6
- 239000002893 slag Substances 0.000 claims description 5
- 108090001060 Lipase Proteins 0.000 claims description 4
- 239000004367 Lipase Substances 0.000 claims description 4
- 102000004882 Lipase Human genes 0.000 claims description 4
- 230000000694 effects Effects 0.000 claims description 4
- 235000019421 lipase Nutrition 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims description 3
- 102000035195 Peptidases Human genes 0.000 claims description 2
- 108091005804 Peptidases Proteins 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 claims description 2
- 229940040461 lipase Drugs 0.000 claims description 2
- 239000000758 substrate Substances 0.000 claims description 2
- -1 galactase Proteins 0.000 abstract description 3
- 239000013543 active substance Substances 0.000 abstract 1
- 108010019077 beta-Amylase Proteins 0.000 abstract 1
- 238000010298 pulverizing process Methods 0.000 abstract 1
- 235000017709 saponins Nutrition 0.000 description 22
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 239000000203 mixture Substances 0.000 description 4
- 108090000623 proteins and genes Proteins 0.000 description 4
- 102000004169 proteins and genes Human genes 0.000 description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 244000061456 Solanum tuberosum Species 0.000 description 2
- 235000002595 Solanum tuberosum Nutrition 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000012043 crude product Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 229930182478 glucoside Natural products 0.000 description 2
- 150000008131 glucosides Chemical class 0.000 description 2
- 150000004676 glycans Chemical class 0.000 description 2
- 210000003734 kidney Anatomy 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000000344 soap Substances 0.000 description 2
- 150000005856 steroid saponins Chemical class 0.000 description 2
- 235000013311 vegetables Nutrition 0.000 description 2
- 239000004382 Amylase Substances 0.000 description 1
- 102000013142 Amylases Human genes 0.000 description 1
- 108010065511 Amylases Proteins 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- 150000003797 alkaloid derivatives Chemical class 0.000 description 1
- 235000019418 amylase Nutrition 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 238000004440 column chromatography Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 235000013409 condiments Nutrition 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000857 drug effect Effects 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 235000019439 ethyl acetate Nutrition 0.000 description 1
- 229930003944 flavone Natural products 0.000 description 1
- 150000002213 flavones Chemical class 0.000 description 1
- 235000011949 flavones Nutrition 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 235000015110 jellies Nutrition 0.000 description 1
- 239000008274 jelly Substances 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 210000001161 mammalian embryo Anatomy 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 1
- 235000019198 oils Nutrition 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 235000018102 proteins Nutrition 0.000 description 1
- 244000017160 saligot Species 0.000 description 1
- 235000009165 saligot Nutrition 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 235000000346 sugar Nutrition 0.000 description 1
- 150000008163 sugars Chemical class 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 208000001072 type 2 diabetes mellitus Diseases 0.000 description 1
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Abstract
A process for extracting saponin from the seeds of common feungreek includes such steps as degumming, defatting, pulverizing, extracting in the aqueous solution containing active substances, such as seminase, galactase, beta-amylase, cellulase, etc. at 40-80 deg.c for 20-48 hr while stirring, and adsorbing by macroreticular resin. Its advantages are low cost and high output rate (0.8-1.5%).
Description
Technical field
The present invention relates to the saponin extracting method, relate in particular to a kind of utilization from the fenugreek seed desugar, the residuum after the degreasing adopts the aqueous solution that is mixed with actives, successfully extracts the method for saponin in the fenugreek seed that saponin is extracted.
Background technology
Semen Trigonellae has another name called Lu Bazi, is the mature seed of annual leguminous herbaceous plant.It is warm in nature, and bitter has warm kidney yang, the effect of dispelling cold and dampness.Recently treat type ii diabetes with Semen Trigonellae, obtain effect preferably.The diabetics takes for a long time and does not find the toxic effect of liver kidney.China medicine office has listed Semen Trigonellae in one of medicinal material as healthcare products.
Semen Trigonellae not only is used as medicine, and also can eat simultaneously, feeding and industrial purposes.It is to have the very cash crop of high value, and all there is plantation all parts of the country.
The structure of fenugreek seed is divided into three layers.Outermost layer is made up of Mierocrystalline cellulose for kind of a skin.And then the middle layer is an endosperm, based on polygalactomannan, accounts for 75%.Innermost layer is an embryo, is made up of effective component, protein, grease etc.Because fenugreek seed exists a large amount of glycan (also claiming vegetable jelly), extract for the drug effect composition and cause difficulty.Domestic existing people's success at present polysaccharide (account for grain weight 28%) from fenugreek seed is peeled off out (seeing patent CN1045304C).But its residue also contains effective components such as small amounts of sugars, vegetables oil, protein and saponin, flavones, alkaloid.
The present invention utilizes desugar exactly, and the residuum after the degreasing adopts the aqueous solution that is mixed with actives, successfully saponin is extracted.
American in 1945 proves contains steroid saponin in the Semen Trigonellae, mainly contain potato saponin, Ya Mu, water caltrop take off, for accuse, new for 8 kinds of steroid saponins such as announcements, wherein the potato saponin accounts for about 85%.Traditional saponin that extracts from Semen Trigonellae adopts solvent method, promptly come unstuck, the granulated slag after the degreasing is with methyl alcohol or extraction using alcohol, concentrate methyl alcohol (or ethanol) medicinal extract (14%), be suspended in the water, after normal hexane, chloroform and acetic ester extraction, its aqueous solution n-butanol extraction reclaims propyl carbinol and promptly gets total saponin.For obtaining pure single saponin, then must receive saponin wash-out one by one and come out through column chromatography, obtain single genuine soap glucoside.
The method of the total saponin of said extracted, the consumption quantity of solvent is big, and three-four kinds of solvents uses by turns, is not suitable for industrial production.
Summary of the invention
The objective of the invention is in order to solve the deficiency that the above-mentioned background technology exists, propose a kind of with low costly, that can realize suitability for industrialized production fully comes unstuck, extracts the granulated slag after the degreasing method of saponin from fenugreek seed.
The objective of the invention is to be achieved through the following technical solutions: the method for extracting saponin in a kind of fenugreek seed, it is characterized in that this method will be come unstuck, the granulated slag of fenugreek seed after the degreasing, with the aqueous solution that contains actives 40 ℃ of temperature--80 ℃, extraction time 20-48 hour, under stirring velocity 30-200 rev/min the effect, and obtain the saponin extracting solution, through big aperture resin absorption, after obtain pure saponin, described actives is a seminase, any 2-4 kind in galactase, the enzyme of washing, saccharifying enzyme, cellulase, lipase and the proteolytic enzyme.
In such scheme, described actives adds concentration between 0.5-8%, and each enzyme optimum addition is the 0.5-4% of substrate.
In such scheme, described during with the actives extraction with aqueous solution optimum temps at 45 ℃--between 60 ℃.
In such scheme, the Best Times of described extraction Semen Trigonellae saponin is between 24-38 hour.
In such scheme, during described extraction best mixing speed be 80-100 change/hour.
The present invention adopts the water law of adding actives to extract, and can reduce cost significantly, and yield is suitable for suitability for industrialized production between 0.8-1.5%.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Operational path of the present invention is seen Fig. 1.
Embodiment 1: the degreasing granulated slag 1500g that comes unstuck, add 6 times water, and add seminase, amylase, each 22.5g of cellulase in mix, 45 ℃ of insulations 30 hours down, slowly stir (80 rev/mins), after reaction finishes, centrifugation.Solid residue is a protein.Water liquid upper prop (101 type wide aperture resin column), washing, back alcohol wash-out.Behind the recovered alcohol saponin crude product 30.5g, recrystallizing methanol once pure product 17.5g (MP152-155 ℃).
Embodiment 2: come unstuck, degreasing Semen Trigonellae powder 1500g, add 6 times of water, add galactase, saccharification, cellulase, each 30g of lipase in mixture, be incubated 28 hours down at 50 ℃, stir (100 rev/mins), reaction finishes, the about aqueous solution upper prop of centrifugation (101 type wide aperture resin column).Use ethanol elution, collect ethanol liquid after, recovered alcohol, total saponin crude product 41g, recrystallizing methanol once approximately pure product 22.5g (MP:152-155 ℃)
Embodiment 3: the Semen Trigonellae powder 1500g of the degreasing of coming unstuck, add 6 times of water, and add lipase, each 10g of cellulase in mixture, be incubated 30 hours down at 50 ℃, 80 rev/mins of rotating speeds stir, after question response finishes, centrifugation, water liquid upper prop (101 type wide aperture resin) after washing is clean, is used the alcohol wash-out, collect elutriant, recovered alcohol, evaporate to dryness approximately thick saponin 25g, recrystallizing methanol gets 10.8g genuine soap glucoside (MP:152-155 ℃).
The foregoing description can obtain protein 400-500g when separating saponin.Its content is 54-58%, can be used for food, can be used for condiment after the hydrolysis.
Claims (5)
1, extracts the method for saponin in a kind of fenugreek seed, it is characterized in that this method will be come unstuck, the granulated slag of fenugreek seed after the degreasing, with the aqueous solution that contains actives 40 ℃ of temperature--80 ℃, extraction time 20--48 hour, under stirring velocity 30-200 rev/min the effect, and obtain the saponin extracting solution, obtain pure saponin after big aperture resin absorption, described actives is a seminase, any 2-4 kind in galactase, the enzyme of washing, saccharifying enzyme, cellulase, lipase and the proteolytic enzyme.
2, according to the method for extracting saponin in the described fenugreek seed of claim 1, it is characterized in that described actives adds concentration between 0.5--8%, each enzyme optimum addition is the 1.5--4% of substrate.
3, according to the method for extracting saponin in the described fenugreek seed of claim 1, it is characterized in that described during with the actives extraction with aqueous solution optimum temps at 45 ℃--between 60 ℃.
4, according to the method for extracting saponin in the described fenugreek seed of claim 1, the Best Times that it is characterized in that described extraction Semen Trigonellae saponin is between 24-38 hour.
5, according to the method for extracting saponin in the described fenugreek seed of claim 1, when it is characterized in that described extractions best mixing speed be the 80--100 commentaries on classics/hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03118627 CN1456570A (en) | 2003-02-18 | 2003-02-18 | Extraction of saponin from seeds of trigonella foenum-graecum |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03118627 CN1456570A (en) | 2003-02-18 | 2003-02-18 | Extraction of saponin from seeds of trigonella foenum-graecum |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1456570A true CN1456570A (en) | 2003-11-19 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 03118627 Pending CN1456570A (en) | 2003-02-18 | 2003-02-18 | Extraction of saponin from seeds of trigonella foenum-graecum |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1456570A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100360145C (en) * | 2005-08-25 | 2008-01-09 | 吉林大学 | Fenugreek extract and its preparation method and application |
| CN102014942B (en) * | 2008-05-13 | 2012-09-19 | 赛图彼奥有限公司 | Fenugreek extract for treating human and animal diseases involving flagellate parasites |
| CN102816253A (en) * | 2012-09-11 | 2012-12-12 | 西北师范大学 | Method for extracting bottle gourd Pakistan rubber by dual-enzyme coupling |
| CN101089166B (en) * | 2006-06-12 | 2013-06-05 | 罗海章 | Natural enzymolysis process of trigonella seed |
-
2003
- 2003-02-18 CN CN 03118627 patent/CN1456570A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100360145C (en) * | 2005-08-25 | 2008-01-09 | 吉林大学 | Fenugreek extract and its preparation method and application |
| CN101089166B (en) * | 2006-06-12 | 2013-06-05 | 罗海章 | Natural enzymolysis process of trigonella seed |
| CN102014942B (en) * | 2008-05-13 | 2012-09-19 | 赛图彼奥有限公司 | Fenugreek extract for treating human and animal diseases involving flagellate parasites |
| CN102988464A (en) * | 2008-05-13 | 2013-03-27 | 赛图彼奥有限公司 | Fenugreek extract for treating human and animal diseases involving flagellate parasites |
| CN102988464B (en) * | 2008-05-13 | 2014-10-22 | 赛图彼奥有限公司 | Application of Fenugreek extract in preparation of composition comprising Fenugreek water extract and excipient |
| CN102816253A (en) * | 2012-09-11 | 2012-12-12 | 西北师范大学 | Method for extracting bottle gourd Pakistan rubber by dual-enzyme coupling |
| CN102816253B (en) * | 2012-09-11 | 2014-04-16 | 西北师范大学 | Method for extracting fenugreek gum by dual-enzyme coupling |
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