CN1040592A - From pressed cake of camellia seeds, extract the process for purification of saponin - Google Patents
From pressed cake of camellia seeds, extract the process for purification of saponin Download PDFInfo
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- CN1040592A CN1040592A CN 89105715 CN89105715A CN1040592A CN 1040592 A CN1040592 A CN 1040592A CN 89105715 CN89105715 CN 89105715 CN 89105715 A CN89105715 A CN 89105715A CN 1040592 A CN1040592 A CN 1040592A
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- saponin
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- pressed cake
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Abstract
The process for purification that extracts saponin from pressed cake of camellia seeds belongs to the accessory product of grain and oil process for purification.
Be widely used in the refining of tea saponin and sasanguasaponin, particularly be applicable to the process for purification that extracts saponin from the industry oil tea-cake dregs, it not only improves the purity and the whiteness of saponin greatly, and can increase substantially the economic benefit of camellia grouts comprehensive utilization.
Description
The invention belongs to grain and oil and pay the process for purification of product.
Tea saponin and sasanguasaponin all belong to and extract in the grouts after the plant of theaceae seed shells, extracts oil and get.It is a kind of good natural nonionic surface active agent, have certain physiologically active, emulsification, dispersion and performance such as moistening, and the pharmacological action of aspects such as impervious, anti-inflammatory, analgesia is arranged, therefore, be widely used in industries such as light industry, chemical industry, weaving, medicine.Sasanguasaponin emulsifying agent, whipping agent, washing composition, the agricultural chemicals etc. done commonly used.But used sasanguasaponin is a kind of raw product at present, contains impurity, color depths such as plant pigments, and application is restricted.In order to apply, must make with extra care.According to " Zhejiang science and technology of grain and oil ", the tea saponin extracting method of 1979 1 phase P6 report " Japan occupies oiling Industrial Co., Ltd just " is as follows: 1, with the grouts after the shelling of tea seed, the oil expression as raw material; 2, after the degreasing, extract out, add ether again tea saponin precipitation is separated out with methyl alcohol; 3, throw out is obtained filbert thick saponin powder by filtration, drying, pulverizing.The refining of it is to adopt the plumbic acetate precipitator method, makes crystallization tea saponin, and the rate of recovery only is 50～60% of a thick saponin.In order to make the purity height, the saponin that color is more shallow the 7th page of above-mentioned data, has also been introduced with the method for chlorinated lime bleaching and has been made with extra care thick saponin, though this method can make whiter saponin fine powder simultaneously.But there is following shortcoming in it: 1, increased the inorganic salt impurity in the saponin; 2, make the water-soluble reduction of saponin; 3, chlorinated lime in use, decomposing the chlorine emit has corrosive nature to equipment, toxic to the people, and environment is brought serious pollution." Chinese Hospitals pharmaceutical journal " 1986 the 6th the 9th phases of volume have been reported in " research (one) of the anti-superficial mycosis activeconstituents of tea seed cake " that the Tang Xiang of plant teaching and research room of Hubei College Of Traditional Chinese Medicine is happy, clear two comrades of Lu Jin deliver, having introduced a kind of is raw material with the thick saponin that extracts in the grouts after tea seed shelling, the oil expression, the employing chromatography is refining, technology is as follows: 1, with cold putting behind the thick saponin of dissolve with ethanol of heat 95%, separate out a large amount of white things, filter collection precipitation; 2, throw out is repeatedly washed through 95% ethanol, get the canescence thing; 3, throw out is again through CHCl
3: CH
2OH behind 7: 2 the eluant solution, continues and uses CHCl
3: CH
2OH is 2: 1 a eluant solution, uses CHCl again
3: CH
2OH is 1: 1 a eluant solution, be recycled to dried, 4, again with molten cold the putting of 95% hot ethanol, separate out after a large amount of white things filter, use 95% ethanol periodic crystallisation at last, promptly get white saponin.This method not only expends a large amount of organic solvents, and complex process, the operational condition harshness, and the cycle is long, and the rate of recovery only accounts for 2.8% of thick saponin." medicinal herb components chemistry " book P450-451 that Chinese science press published in 1977, introduced the process for purification of five kinds of saponins altogether, promptly 1, magnesium oxide adsorbing method, 2, the hydrated barta precipitator method, 3, aluminum hydroxide precipitation method, 4, mantoquita method, 5, two-phase solvent extraction method.Yet, present industrial Theaceae grouts, particularly cake of camellia oleifera seeds is to get with the tea seed oil expression back of not shelling, this grouts claim that again tea is withered, people commonly used it make fertilizer, if extract thick saponin with it, it is many wherein to contain impurity such as plant pigments, color is dark-brown or brown, and application is restricted.If use above-mentioned process for purification, all can not improve the purity and the whiteness of saponin, this is proved by repeatedly testing.
The objective of the invention is, provide a kind of technology simple, easy to operate, cost is low, rate of recovery height, the process for purification of non-environmental-pollution again.The raw material of this process for purification is the thick saponin that extracts the grouts after the Theaceae seed does not shell, extracts oil.
Technical scheme of the present invention is such: the thick saponin that extracts from pressed cake of camellia seeds, its composition are complicated, and color is dark-brown or brown.Pure product saponin should be white.Adopt above-mentioned process for purification all can not obtain pure product saponin, we at first carry out careful analysis to the performance and the contained major impurity of raw material thus, through repeatedly qualitative analysis and quantitative analysis, confirm that contained major impurity is phenolic substances such as flavonoid compound in the raw material (thick saponin).Because its existence directly affects the application of saponin, improve the purity and the whiteness of thick saponin, must remove phenolic substances such as flavonoid compound.In view of flavonoid compound comparatively close with the saponin solubility property.As adopt classical conventional separation method, and be of no avail as separation such as the solvent method or the precipitator method, and for example adopt the chlorinated lime bleaching process, experimental result proof product still is a brown.Adopt chromatography for another example, can separate effectively, also can obtain, but technical process is long than straight product, the conditional request height, trivial operations, the rate of recovery is low, the cost height.From economic angle, should not adopt.The substantial technical characterstic of the present invention adopts the finishing agent decomposition method exactly, promptly adds the molecular structure that finishing agent destroyed and decomposed flavonoid compound in thick saponin, thereby obtains refining saponin.This process for refining is simple, need not separation means and specific installation, and the rate of recovery can surpass 90%, and cost is low, does not have advantages such as waste water, waste residue and environmental pollution again.This method is not only technical feasible, but also can obtain the product of different purity according to the needs in market.Therefore, can be widely used in the comprehensive utilization of pressed cake of camellia seeds on the current industrial, particularly cake of camellia oleifera seeds, improve the economic benefit of grouts widely.
Accompanying drawings process for refining feature of the present invention is as follows:
A, do not shell with the plant of theaceae seed, in the grouts after the oil expression, the thick saponin of extraction is purified raw material (3);
B, finishing agent: promptly use neutralizing agent (1) to join in the finishing agent (2), stir, and modulate PH=8～9 of solution, perhaps add 0.1～0.3 complexing agent again in above-mentioned modulation solution, perhaps finishing agent (2) uses separately;
C, finishing agent is joined in the raw material (3), the ratio of adjusting solid and liquid is 1: 0.5～1, evenly stirs into pulpous state then;
D, drying: drying temperature is controlled at below 110 ℃, 75～110 ℃ of optimum tempss.The exsiccant method can be common blowing-type oven method, also can adopt the desiccating method of Kun cartridge type, also can adopt spray-drying process.
E, packing: since the easy moisture absorption of saponin, the packing instructions weather-proof dressing.
Because it is responsive that saponin all compares acid, alkali and oxygenant, so the finishing agent that adds is the more weak oxygenant of a kind of oxidation susceptibility, as S-WAT or hydrogen peroxide.Neutralizing agent (1) can be caustic alkali or clorox or Losantin.The consumption of neutralizing agent (1) is 1%～1.5% of a finishing agent.If in finishing agent (2), add 0.1%～0.3% complexing agent, more can help to improve the whiteness of product, the complexing agent that adopts is a disodium ethylene diamine tetraacetate usually.
Description of drawings: (1) neutralizing agent, (2) finishing agent, (3) raw material, (4) condiment slurrying, (5) dry, (6) packing.
Embodiment 1:
Getting and extract whiteness from cake of camellia oleifera seeds is 1 kilogram of the 17 thick saponin of spending, and adds 0.25 kilogram in hydrogen peroxide, normal-temperature operation, constantly stir, making the solid and the ratio of liquid is 1: 0.5, and the pulp that stirs, and then soup compound is sent into the oven drying of blowing-type to doing.Its oven temperature is 75～110 ℃, can obtain 0.926 kilogram refined saponin, and the rate of recovery reaches 92.6%, and its whiteness is 39.7 degree.
Embodiment 2:
Get from cake of camellia oleifera seeds 1 kilogram of the thick saponin that extracts whiteness, finishing agent is with 0.25 kilogram in hydrogen peroxide, again with in sodium hydroxide 0.68 gram and hydrogen peroxide, make solution PH=8～9, slowly join in the thick saponin again, and constantly stir into pulpous state, then soup compound is sent into the blowing-type oven drying to doing.Its oven temperature is 75～110 ℃ can get 0.937 kilogram of refined saponin, and the rate of recovery reaches 93.7%, and its whiteness is 40.2 degree.
Claims (5)
1, from pressed cake of camellia seeds, extract the process for purification of saponin, it is characterized in that:
A, do not shell with the plant of theaceae seed, in the grouts after the oil expression, the thick saponin of proposition is raw material (3);
B, finishing agent: promptly use neutralizing agent (1) to join in the finishing agent (2), stir, and PH=8～9 of modulation solution, perhaps in above-mentioned modulation solution, add complexing agent again, perhaps finishing agent (2) uses separately;
C, finishing agent is joined in the raw material (3), the ratio of adjusting solid and liquid is 1: 0.5～1 evenly to stir into pulpous state then;
D, drying;
E, packing.
2, the process for purification that from pressed cake of camellia seeds, extracts saponin according to claim 1, it is characterized in that finishing agent (2) adopts the more weak oxygenant of oxidation susceptibility, neutralizing agent (1) is caustic alkali or clorox, perhaps Losantin, and complex compound is disodium ethylene diamine tetraacetate (EDTA);
3, extract the process for purification of saponin in the pressed cake of camellia seeds according to claim 1 and 2, it is characterized in that more weak oxygenant can be hydrogen peroxide or S-WAT;
4, the process for purification that extracts saponin from pressed cake of camellia seeds according to claim 1 is characterized in that drying temperature below 110 ℃, and optimum temps is 75-110 ℃.
5, according to claim 1 or the 4 described process for purification that from pressed cake of camellia seeds, extract saponin, it is characterized in that the exsiccant method can adopt the oven method of common blowing-type, also can adopt the desiccating method of Kun cartridge type, can also adopt spray-drying process.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 89105715 CN1026114C (en) | 1989-05-06 | 1989-05-06 | Method of refining saponin extracted from waste pressed cake of camellia seeds |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 89105715 CN1026114C (en) | 1989-05-06 | 1989-05-06 | Method of refining saponin extracted from waste pressed cake of camellia seeds |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1040592A true CN1040592A (en) | 1990-03-21 |
| CN1026114C CN1026114C (en) | 1994-10-05 |
Family
ID=4856365
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 89105715 Expired - Fee Related CN1026114C (en) | 1989-05-06 | 1989-05-06 | Method of refining saponin extracted from waste pressed cake of camellia seeds |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1026114C (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1058971C (en) * | 1995-02-11 | 2000-11-29 | 国内贸易部西安油脂科学研究设计院 | Prodn. technology for extracting fine sasanquasaponin by super filtration film method |
| CN1061352C (en) * | 1997-01-24 | 2001-01-31 | 中国科学院化学研究所 | Extraction method of oil-tea camellia seed saponin |
| CN101863949A (en) * | 2010-05-25 | 2010-10-20 | 青田中野天然植物科技有限公司 | Structural modification type cameclia oleifera saponin and preparation method and application thereof |
| CN101906296A (en) * | 2010-05-25 | 2010-12-08 | 青田中野天然植物科技有限公司 | Camellia saponin type oilfield foaming agent and preparation method and application thereof |
| CN113248552A (en) * | 2021-05-21 | 2021-08-13 | 广州德谷个人护理用品有限公司 | Method for extracting and decoloring tea saponin |
| CN115286681A (en) * | 2022-08-04 | 2022-11-04 | 湖南朗林生物资源股份有限公司 | Preparation method of tea saponin extract |
-
1989
- 1989-05-06 CN CN 89105715 patent/CN1026114C/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1058971C (en) * | 1995-02-11 | 2000-11-29 | 国内贸易部西安油脂科学研究设计院 | Prodn. technology for extracting fine sasanquasaponin by super filtration film method |
| CN1061352C (en) * | 1997-01-24 | 2001-01-31 | 中国科学院化学研究所 | Extraction method of oil-tea camellia seed saponin |
| CN101863949A (en) * | 2010-05-25 | 2010-10-20 | 青田中野天然植物科技有限公司 | Structural modification type cameclia oleifera saponin and preparation method and application thereof |
| CN101906296A (en) * | 2010-05-25 | 2010-12-08 | 青田中野天然植物科技有限公司 | Camellia saponin type oilfield foaming agent and preparation method and application thereof |
| CN101906296B (en) * | 2010-05-25 | 2013-04-24 | 青田中野天然植物科技有限公司 | Camellia saponin type oilfield foaming agent and preparation method and application thereof |
| CN101863949B (en) * | 2010-05-25 | 2013-07-24 | 青田中野天然植物科技有限公司 | Structural modification type cameclia oleifera saponin and preparation method and application thereof |
| CN113248552A (en) * | 2021-05-21 | 2021-08-13 | 广州德谷个人护理用品有限公司 | Method for extracting and decoloring tea saponin |
| CN115286681A (en) * | 2022-08-04 | 2022-11-04 | 湖南朗林生物资源股份有限公司 | Preparation method of tea saponin extract |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1026114C (en) | 1994-10-05 |
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