CN104211749A - Production technology of soapnut saponins - Google Patents
Production technology of soapnut saponins Download PDFInfo
- Publication number
- CN104211749A CN104211749A CN201410400900.5A CN201410400900A CN104211749A CN 104211749 A CN104211749 A CN 104211749A CN 201410400900 A CN201410400900 A CN 201410400900A CN 104211749 A CN104211749 A CN 104211749A
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- CN
- China
- Prior art keywords
- soapnut
- silica gel
- sapindoside
- saponins
- production technique
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 19
- 241000580955 Sapindus mukorossi Species 0.000 title claims abstract description 15
- 229930182490 saponin Natural products 0.000 title claims abstract description 13
- 150000007949 saponins Chemical class 0.000 title claims abstract description 13
- 235000017709 saponins Nutrition 0.000 title abstract description 12
- 238000005516 engineering process Methods 0.000 title abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 18
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000000706 filtrate Substances 0.000 claims abstract description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000000741 silica gel Substances 0.000 claims abstract description 13
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 8
- 230000005526 G1 to G0 transition Effects 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 229930183111 sapindoside Natural products 0.000 claims description 18
- 238000000605 extraction Methods 0.000 claims description 12
- 238000004587 chromatography analysis Methods 0.000 claims description 7
- 238000009826 distribution Methods 0.000 claims description 7
- 239000001397 quillaja saponaria molina bark Substances 0.000 claims description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 4
- 239000012467 final product Substances 0.000 claims description 2
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 2
- 239000003814 drug Substances 0.000 abstract description 3
- 230000002378 acidificating effect Effects 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 238000005406 washing Methods 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 abstract 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract 1
- 229910052799 carbon Inorganic materials 0.000 abstract 1
- 229940079593 drug Drugs 0.000 abstract 1
- 238000005192 partition Methods 0.000 abstract 1
- 238000004810 partition chromatography Methods 0.000 abstract 1
- 238000000746 purification Methods 0.000 abstract 1
- 238000002137 ultrasound extraction Methods 0.000 abstract 1
- 238000004140 cleaning Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- IAGSHEHQJJTLLR-FNINEVAMSA-N (4as,6ar,6as,6br,8ar,9r,10s,12ar,14bs)-10-[(2s,3r,4s,5s)-3-[(2s,3r,4r,5s,6s)-3,5-dihydroxy-6-methyl-4-[(2s,3r,4s,5r)-3,4,5-trihydroxyoxan-2-yl]oxyoxan-2-yl]oxy-4,5-dihydroxyoxan-2-yl]oxy-9-(hydroxymethyl)-2,2,6a,6b,9,12a-hexamethyl-1,3,4,5,6,6a,7,8,8a,10, Chemical compound O([C@H]1[C@@H](O)[C@H](O[C@H]2[C@@H](OC[C@H](O)[C@@H]2O)O[C@@H]2[C@@]([C@H]3[C@]([C@@H]4[C@@]([C@@]5(CC[C@]6(CCC(C)(C)C[C@H]6C5=CC4)C(O)=O)C)(C)CC3)(C)CC2)(C)CO)O[C@H]([C@@H]1O)C)[C@@H]1OC[C@@H](O)[C@H](O)[C@H]1O IAGSHEHQJJTLLR-FNINEVAMSA-N 0.000 description 1
- 241000222122 Candida albicans Species 0.000 description 1
- 206010007134 Candida infections Diseases 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 241000590002 Helicobacter pylori Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000000629 anti-dermatophyte Effects 0.000 description 1
- 230000010100 anticoagulation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 201000003984 candidiasis Diseases 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000003480 eluent Substances 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
- 238000005187 foaming Methods 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 229940037467 helicobacter pylori Drugs 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 238000001728 nano-filtration Methods 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000013558 reference substance Substances 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- IAGSHEHQJJTLLR-UHFFFAOYSA-N sapindoside B Natural products OC1C(C)OC(OC2C(OCC(O)C2O)OC2C(C3C(C4C(C5(CCC6(CCC(C)(C)CC6C5=CC4)C(O)=O)C)(C)CC3)(C)CC2)(C)CO)C(O)C1OC1OCC(O)C(O)C1O IAGSHEHQJJTLLR-UHFFFAOYSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000000194 supercritical-fluid extraction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 210000004881 tumor cell Anatomy 0.000 description 1
- 238000003809 water extraction Methods 0.000 description 1
Landscapes
- Medicines Containing Plant Substances (AREA)
- Steroid Compounds (AREA)
- Saccharide Compounds (AREA)
Abstract
The invention belongs to the fields of medicines and chemical industry, and discloses a production technology of soapnut saponins. The technology comprises the following steps: 1, carrying out ultrasonic extraction of soapnut powder by n-butanol, mixing the above obtained filtrates, respectively washing by acidic water and alkaline water, and concentrating until dryness; 2, carrying out silica gel partition chromatography purification by using a silica gel partition chromatographic column with silica gel as a , water as a stationary phase and n-butanol as a mobile phase, eluting, abandoning the obtained early eluate of 0.25BV, collecting later eluates of 4BV, and mixing the collected eluates; and 3, decoloring: taking the eluate obtained in step 2, adding active carbon, carrying out ultrasonic decoloring, filtering, mixing the above obtained filtrates, and concentrating until dryness in order to obtain the soapnut saponins with the purity of 90-95%. The method allows highly pure soapnut saponins to rapidly and simply be obtained from soapnut pulp, adopts routine technologies, has a low cost, and provides a new method for the industrial production of the highly pure soapnut saponins.
Description
Technical field
The present invention relates to field of medicine and chemical technology, be specifically related to a kind of production technique of high purity total saponin of sapindusmukerossi.
Background technology
Sapindoside has anti-dermatophyte, candidiasis and anti Helicobacter pylori activity, is a kind of natural clean rhzomorph, and has the multiple biological activitys such as inhibition tumor cell propagation, anticoagulation, have a good application prospect at field of medicaments.Sapindoside or the tensio-active agent of pure natural, pH value is between 5 ~ 7, and in naturally acid, foaming abundancy, feel is fine and smooth, strong detergency, is the natural washing raw material that cleaning capacity is best in the world.Sapindoside can be degradable, do not hurt sb.'s feelings body, not polluted source, can be used for manufacturing natural nuisance-free cleaning supplies.This class natural phant cleaning supplies, Japan and Korea S and European and American developed countries quite popular.
Present stage, the research of sapindoside production technique, still rests on the extraction stage to a great extent, rarely carries out follow-up study.Chinese patent CN 102617695 B discloses a kind of production technique of sapindoside, and purity can reach 90%.But the method relates to supercritical extraction, nanofiltration, the technology such as spraying dry, make troubles to industrial production.
Summary of the invention
The object of the invention is to, by extracting, concentrate, decolouring, a series of routine operations such as precipitation, do not relate to complex instrument and technology, and can obtain the sapindoside of purity 90%-95%, color is pure white, are conducive to subsequent production and exploitation.
The present invention is directed to the complex manufacturing of existing sapindoside, be unfavorable for the defect of suitability for industrialized production, a kind of simple and sapindoside production technique that product purity is high is provided.
Object of the present invention is achieved through the following technical solutions: a kind of production technique of sapindoside, comprises the following steps:
S1. by Seed of Chinese Soapberry powder propyl carbinol supersound extraction, merging filtrate, filtrate is dry with being concentrated into after sour water and soda lye wash respectively;
S2. silica gel distribution chromatography post:
Get S1 gained total saponin of sapindusmukerossi silica gel distribution chromatography purifying, using silica gel as balustrade, using water as stationary phase, using propyl carbinol as moving phase, first wash-out 0.25BV discards, then wash-out 4BV, merges elutriant;
S3. decolour:
Get elutriant under S2, add the ultrasonic decolouring of gac, merging filtrate after filtering, is concentrated into dry, obtains final product.
The add-on of the water described in step S1 is 20 ~ 50 times of Seed of Chinese Soapberry powder volume; Be heated to 70 ~ 100 DEG C.
Supersound extraction described in step S1 refers to extraction 10 ~ 30min under the condition of 30 ~ 50kHz.
Centrifugal described in step S1 or S4 refers to centrifugal 3 ~ 10min under the condition of 2000 ~ 5000r/min.
The add-on of the ultrasonic decolouring of described gac is the 6%-10% of total amount, and the number of times of decolouring is 2-3 time, each 10-30min.
Beneficial effect of the present invention is:
Sapindoside production technique provided by the invention is quick, easy, low cost, the equipment not relating to any complexity and technology; The high purity 90 ~ 95% of product, the pure white exquisiteness of color; Be suitable for subsequent development and production, also for the industrialization of high purity sapindoside provides technical guarantee;
The creationary employing propyl carbinol of present method is as Extraction solvent, reduce the proposition of the impurity such as polysaccharide, tanning in existing alcohol extracting or water extraction process, with impurity such as sour water precipitation tannings, wash away the acidic impurities such as flavones with buck, by simple operations, the total saponins that purity is higher can be obtained;
Using propyl carbinol as eluent, be easy to reclaim, loss is few, is conducive to reducing costs;
Silica gel is cheap, good separating effect, regeneration easily, activity easily controls, and is very suitable for sapindoside purifying.
Embodiment
Explain the present invention further below in conjunction with specific embodiment, but embodiment does not limit in any form to the present invention.Unless stated otherwise, the present invention adopts test method, reagent and equipment are the art ordinary method, reagent and equipment.
Embodiment 1
Get Seed of Chinese Soapberry powder 50g, add 5 times of water-saturated n-butanols, supersound extraction 4 times, each 15min; Filter, merging filtrate is concentrated into dry, and cross silica gel distribution chromatography, using water as stationary phase, propyl carbinol is as moving phase, and front 0.25BV discards, 4BV elutriant after collecting; Elutriant adds the ultrasonic decolouring of gac 2 times of 10%, each 20min, and merging filtrate after filtering, is concentrated into dry, obtains purity more than 90%, the total saponin of sapindusmukerossi 6g that color is pure white.
Embodiment 2
Get Seed of Chinese Soapberry powder 1000g, add 7 times of water-saturated n-butanols, supersound extraction 3 times, each 20min; Filter, merging filtrate is concentrated into dry, crosses silica gel distribution chromatography.Using water as stationary phase, propyl carbinol is as moving phase, and front 0.25BV discards, 4BV elutriant after collecting; Elutriant adds the ultrasonic decolouring of gac 3 times of 6%, each 15min, and merging filtrate after filtering, is concentrated into dry, obtains purity more than 90%, the total saponin of sapindusmukerossi 12g that color is pure white.
Embodiment 3
Get Seed of Chinese Soapberry powder 250g, add 6 times of water-saturated n-butanols, supersound extraction 4 times, each 30min; Filter, merging filtrate is concentrated into dry, and cross silica gel distribution chromatography, using water as stationary phase, propyl carbinol is as moving phase, and front 0.25BV discards, 4BV elutriant after collecting; Elutriant adds the ultrasonic decolouring of gac 2 times of 10%, each 20min, and merging filtrate after filtering, is concentrated into dry, obtains the total saponin of sapindusmukerossi 30g that purity more than 90% color is pure white.
Note: UV purity detecting use reference substance to be in Seed of Chinese Soapberry to be separated the saponin(e sapindoside B obtained.
Claims (5)
1. a production technique for sapindoside, is characterized in that, comprises the following steps:
S1. by Seed of Chinese Soapberry powder propyl carbinol supersound extraction, merging filtrate, filtrate is dry with being concentrated into after sour water and soda lye wash respectively;
S2. silica gel distribution chromatography post:
Get S1 gained total saponin of sapindusmukerossi silica gel distribution chromatography purifying, using silica gel as balustrade, using water as stationary phase, using propyl carbinol as moving phase, first wash-out 0.25BV discards, then wash-out 4BV, merges elutriant;
S3. decolour:
Get elutriant under S2, add the ultrasonic decolouring of gac, after filtering, merging filtrate is concentrated into dry, to obtain final product.
2. the production technique of sapindoside according to claim 1, is characterized in that, the add-on of the propyl carbinol described in step S1 is 5 ~ 8 times of Seed of Chinese Soapberry powder volume; The number of times of supersound extraction is 2 ~ 3 times.
3. the production technique of sapindoside according to claim 1, is characterized in that, the supersound extraction described in step S1 refers to extraction 10 ~ 30min under the condition of 30 ~ 50kHz.
4. the production technique of sapindoside according to claim 1, is characterized in that, centrifugal described in step S1 or S4 refers to centrifugal 3 ~ 10min under the condition of 2000 ~ 5000r/min.
5. the production technique of sapindoside according to claim 1, is characterized in that, the add-on of the ultrasonic decolouring of described gac is the 6%-10% of total amount, and the number of times of decolouring is 2-3 time, each 10-30min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410400900.5A CN104211749B (en) | 2014-08-15 | 2014-08-15 | A kind of production technology of sapindoside |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410400900.5A CN104211749B (en) | 2014-08-15 | 2014-08-15 | A kind of production technology of sapindoside |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104211749A true CN104211749A (en) | 2014-12-17 |
| CN104211749B CN104211749B (en) | 2016-08-24 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410400900.5A Active CN104211749B (en) | 2014-08-15 | 2014-08-15 | A kind of production technology of sapindoside |
Country Status (1)
| Country | Link |
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| CN (1) | CN104211749B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104744555A (en) * | 2015-04-09 | 2015-07-01 | 成都市三禾田生物技术有限公司 | Method for extracting and separating sapindoside B from plant natural saponine soapberries |
| CN104840387A (en) * | 2015-04-28 | 2015-08-19 | 百朗德生物化学海门有限公司 | Low-irritation-smell soapberry fruit extract production method |
| CN113546574A (en) * | 2021-06-23 | 2021-10-26 | 广东菁萃生物科技有限公司 | High-stability saponin composition and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101624416A (en) * | 2008-07-07 | 2010-01-13 | 中国林业科学研究院亚热带林业研究所 | Method of separating soapnut saponin with foam separation method |
| CN102038793A (en) * | 2010-09-27 | 2011-05-04 | 南京泽朗医药科技有限公司 | Preparation method of soapberry saponin |
-
2014
- 2014-08-15 CN CN201410400900.5A patent/CN104211749B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101624416A (en) * | 2008-07-07 | 2010-01-13 | 中国林业科学研究院亚热带林业研究所 | Method of separating soapnut saponin with foam separation method |
| CN102038793A (en) * | 2010-09-27 | 2011-05-04 | 南京泽朗医药科技有限公司 | Preparation method of soapberry saponin |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104744555A (en) * | 2015-04-09 | 2015-07-01 | 成都市三禾田生物技术有限公司 | Method for extracting and separating sapindoside B from plant natural saponine soapberries |
| CN104840387A (en) * | 2015-04-28 | 2015-08-19 | 百朗德生物化学海门有限公司 | Low-irritation-smell soapberry fruit extract production method |
| CN113546574A (en) * | 2021-06-23 | 2021-10-26 | 广东菁萃生物科技有限公司 | High-stability saponin composition and application thereof |
| WO2022268235A1 (en) * | 2021-06-23 | 2022-12-29 | 广东菁萃生物科技有限公司 | Saponin composition having high stability and use thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104211749B (en) | 2016-08-24 |
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