CN101817853A - Method for extracting tea saponin by adopting tea seed cake - Google Patents
Method for extracting tea saponin by adopting tea seed cake Download PDFInfo
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- CN101817853A CN101817853A CN200910021714A CN200910021714A CN101817853A CN 101817853 A CN101817853 A CN 101817853A CN 200910021714 A CN200910021714 A CN 200910021714A CN 200910021714 A CN200910021714 A CN 200910021714A CN 101817853 A CN101817853 A CN 101817853A
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Abstract
The invention relates to a method for extracting tea saponin by adopting a tea seed cake, comprising the following steps of: firstly smashing a dry tea seed cake after tea seed oil is extracted, and then placing into a reaction vessel; adding the petroleum ether with the mass concentration of 90-95 percent according to a proportion of the mass/volume ratio of 1:3, and stirring at constant temperature for reaction at the temperature of 55 DEG C to carry out derosination for 1 hours, and filtering after the reaction, wherein the mass of tea seed powder is expressed as grams and the volume of petroleum ether is expressed as ml;; drying filtered filter residues, and then placing into the reaction vessel; adding ethanol with the mass concentration of 80-95 percents according to the proportion of the mass ratio of 1:5-7, and stirring to carry out reflux extraction at 65-75 DEG C by two times for 1.5-3.5 hours, and filtering filter liquor when the filter liquor is hot; distilling the filter liquor, and concentrating to one tenth of original volume at temperature which is not higher than 60 DEG C; adding acetone equivalent to two times of the liquid volume of concentrated liquor to the concentrated liquor for extraction, wherein faint yellow sediments are generated during the extraction; and carrying out vacuum drying on filter residues to obtain faint yellow rough saponin at normal temperature or low temperature.
Description
Technical field
The present invention relates to a kind of preparation method who in tea seed cake, uses extraction using alcohol acetone extract tea saponin nonionogenic tenside, promptly a kind of preparation method of green surfactant tea saponin.
Background technology
Tea saponin is to extract a class Pentacyclic triterpene saponins material from plant of theaceae seed or leaf, is a kind of pure natural saponin.Be nonionic surface active agent, have the performance of emulsification, dispersion, moistening, foaming, pharmacological actions such as impervious, anti-inflammatory, analgesia are arranged, and sterilizing pesticide is arranged and stimulate the function of certain plants growth.It is widely used: at industrial grease-removing agent, emulsifying agent and the anti-friction composition etc. of being used as; Be used for making washing composition and shampoo, the incomparable advantage of other synthetic is arranged; Its pure product pharmaceutically can be used as the medicine for the treatment of diarrhoea, oedema and old trachitis; On agricultural, can be used as desinsection, sterilant and inert ingredient.Looking into saponin in addition is a kind of pure natural saponin, and higher organism is not all had toxic action, so tea saponin meets present consumption idea as a kind of green saponin, development prospect is very wide.
For producing of tea saponin, China just has the people to extract tea saponin with water seaoning in tea seed and leaf as far back as the fifties; Make digestion agent with aqueous methanol or aqueous ethanol, also add lower alcohol auxiliary reagents such as propyl carbinol sometimes with Pentyl alcohol; As digestion agent, in digestion agent, add precipitation agent CaO with hot water, make tea saponin transfer precipitation to, separate with impurity; As digestion agent, then in vat liquor, add flocculating agent A 1 with hot water
2(SO
4)
3, after the precipitation removal of impurities cooling, change collection with 95% ethanol again and purify; Macroporous resin is the class organic high molecular polymer that development in recent years is got up.Produce at existing Chinese patent H0302, MD0301, G0302,200610128258 (application number) etc. and to be reported that in the process that still for the last crystallization of tea saponin, major part has all adopted the high vacuum-drying of consuming energy.The present invention utilizes tea saponin should not be dissolved in the rerum natura of acetone, tea saponin directly extracted in extracting solution, and dry at normal temperatures being worth, technology is simple, and energy expenditure is low.
Summary of the invention
The purpose of this invention is to provide a kind of method that adopts tea seed cake extraction tea saponin.
The present invention is a kind of method that adopts tea seed cake extraction tea saponin: choose the dried tea seed cake that pressed tea-seed oil, at first use ether defatting, being that solvent directly extracts tea saponin in the degreasing tea seed cake with ethanol again, is extraction in 2: 1 with acetone and concentrated solution volume ratio, the steps include:
(1) at first utilizes the dried tea seed cake that will press tea-seed oil to pulverize, cross 40～60 mesh sieves;
(2) above-mentioned tea powder of seeds is put into reaction vessel, tea powder of seeds quality is in gram, the volume of sherwood oil is in ml, in the quality volumetric ratio is that to add mass concentration be 90%～95% sherwood oil for 1: 3 ratio, under 55 ℃ temperature, carry out the constant temperature stirring reaction, carry out degreasing, time remaining 1 hour, after-filtration is finished in reaction;
(3) will put into above-mentioned reaction vessel after the filter residue and drying after the above-mentioned filtration, in mass ratio be 1: 5～7 ratio to add mass concentration be 80%～95% ethanol, stirring and refluxing leaching 1.5～3.5 hours at twice under 65～75 ℃, filtered while hot filtrate;
(4) filtrate is distilled, concentrate not being higher than under 60 ℃ the temperature, be concentrated to 1/10 of original volume;
(5) add the acetone that is equivalent to 2 times of its liquid volumes in concentrated solution and extract, extraction produces faint yellow precipitation, after the filtration, filter residue is carried out vacuum-drying under normal temperature or low temperature, gets faint yellow thick saponin.
The thick tea saponin of above-mentioned gained is added in the entry, be configured to 3% tea saponin solution, it is composite that tea saponin solution and liquid detergent are pressed mass ratio 1: 9, get compositional liquor to rapeseed oil and machinery oil by the national standard experiment of deoiling, 5% aqueous solution rate of deoiling is respectively 97.1% and 98.9%.
Usefulness of the present invention is: acetone is used for direct extraction, has avoided the aftertreatment complicated technology, and simple, the easy row of these class methods directly utilizes tea seed cake to extract, and turns waste into wealth.
Embodiment
Be specific embodiment below
Embodiment 1:
With pulverizer the dried tea seed cake that 200 grams pressed tea-seed oil is smashed, got the tea seed cake powder, cross 40～60 mesh sieves; The tea seed cake powder of 50 grams is put into the reaction vessel being with stirring mechanism, prolong is housed, in this reaction vessel, add the 150ml mass concentration and be 90%～95% sherwood oil, stirring also is heated to 55 ℃, heating was kept 1 hour, react the after-filtration that finishes, filtrate is put into receiving flask.Above-mentioned reaction vessel will be put into after the filter residue and drying, adding 250g concentration is 85% ethanol in this reaction vessel, reaction was stirred 1.5 hours at twice under 75 ℃ of steady temperatures, after-filtration is finished in reaction, filter residue reclaims, filtrate is distilled, concentrate not being higher than under 60 ℃ the temperature, with the filtrate vacuum concentration to 1/10 of original volume, add the acetone that is equivalent to 2 times of its liquid volumes and extract in concentrated solution, extraction produces faint yellow precipitation, after the filtration, filter residue is dry under cryogenic vacuum, get faint yellow tea saponin.
Embodiment 2:
With pulverizer the dried tea seed cake that 200 grams pressed tea-seed oil is smashed, got the tea seed cake powder, cross 40～60 mesh sieves; The above-mentioned powder of 50 grams is put into the reaction vessel that a band stirred, was equipped with prolong, adding 150ml mass concentration is 90%～95% sherwood oil in this container, stirs and be heated to 55 ℃, and heating was kept 1 hour, react the after-filtration that finishes, filtrate is put into receiving flask.Above-mentioned reaction vessel will be put into after the filter residue and drying, add 300g concentration and be 90% ethanol in this container, reaction was stirred 2.5 hours at twice under 75 ℃ of steady temperatures, and after-filtration is finished in reaction, filter residue reclaims, filtrate is distilled, concentrates not being higher than under 60 ℃ the temperature, with the filtrate vacuum concentration to 1/10 of original volume, adding the acetone that is equivalent to 2 times of its liquid volumes in concentrated solution extracts, extraction produces faint yellow precipitation, carries out drying at normal temperature, gets faint yellow tea saponin.
Embodiment 3:
With pulverizer the dried tea seed cake that 200 grams pressed tea-seed oil is smashed, got the tea seed cake powder, cross 40～60 mesh sieves; The above-mentioned powder of 100 grams is put into the reaction vessel that a band stirred, was equipped with prolong, adding 300ml mass concentration is 90%～95% sherwood oil in this container, stirs and be heated to 55 ℃, and heating was kept 1 hour, react the after-filtration that finishes, filtrate is put into receiving flask.Above-mentioned reaction vessel will be put into after the filter residue and drying, add 350g concentration and be 95% ethanol in this container, reaction was stirred 3.5 hours at twice under 75 ℃ of steady temperatures, and after-filtration is finished in reaction, filter residue reclaims, filtrate is distilled, concentrates not being higher than under 60 ℃ the temperature, with the filtrate vacuum concentration to 1/10 of original volume, adding the acetone that is equivalent to 2 times of its liquid volumes in concentrated solution extracts, extraction produces faint yellow precipitation, carries out drying at normal temperature, gets faint yellow tea saponin.
Claims (1)
1. adopt the method for tea seed cake extraction tea saponin: choosing the dried tea seed cake that pressed tea-seed oil, at first use ether defatting, is that solvent directly extracts tea saponin in the degreasing tea seed cake with ethanol again, is extraction in 2: 1 with acetone and concentrated solution volume ratio, the steps include:
(1) at first utilizes the dried tea seed cake that will press tea-seed oil to pulverize, cross 40～60 mesh sieves;
(2) above-mentioned tea powder of seeds is put into reaction vessel, tea powder of seeds quality is in gram, the volume of sherwood oil is in ml, in the quality volumetric ratio is that to add mass concentration be 90%～95% sherwood oil for 1: 3 ratio, under 55 ℃ temperature, carry out the constant temperature stirring reaction, carry out degreasing, time remaining 1 hour, after-filtration is finished in reaction;
(3) filter residue after the above-mentioned filtration is carried out put into above-mentioned reaction vessel after the drying, in mass ratio is that to add mass concentration be 80%～95% ethanol for 1: 5～7 ratio, stirring and refluxing was leached 1.5～3.5 hours at twice under 65～75 ℃, filtered while hot filtrate;
(4) filtrate is distilled, temperature is not higher than under 60 ℃ and concentrates, and is concentrated to 1/10 of original volume;
(5) add the acetone that is equivalent to 2 times of its liquid volumes in concentrated solution and extract, extraction produces faint yellow precipitation, after the filtration, filter residue is carried out vacuum-drying get faint yellow thick saponin under normal temperature or low temperature.
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| CN200910021714A CN101817853A (en) | 2009-03-14 | 2009-03-14 | Method for extracting tea saponin by adopting tea seed cake |
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| CN200910021714A CN101817853A (en) | 2009-03-14 | 2009-03-14 | Method for extracting tea saponin by adopting tea seed cake |
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101967177A (en) * | 2010-09-17 | 2011-02-09 | 华中农业大学 | Extract and method for extracting tea saponin from oil-tea seed residue |
| CN102020692A (en) * | 2010-12-15 | 2011-04-20 | 华中科技大学 | Method for extracting refined tea saponin from camellia oleifera seed cake |
| CN102028042A (en) * | 2010-10-28 | 2011-04-27 | 福建省尤溪县沈郎食用油有限公司 | Method and equipment for preparing tea seed oil from tea seeds and extracting tea polyphenol from byproduct tea seed cake |
| CN102659902A (en) * | 2012-05-02 | 2012-09-12 | 湖南山润油茶科技发展有限公司 | Process for extracting high-purity tea saponin from tea seed cakes |
| CN103509069A (en) * | 2012-06-27 | 2014-01-15 | 上海莱博生物科技有限公司 | Preparation method of crude product of tea saponin and preparation method of tea saponin B1 |
| CN103950639A (en) * | 2014-05-20 | 2014-07-30 | 贵州大学 | Method of storing tea seed pancake by utilizing vacuum package |
| CN104177508A (en) * | 2014-08-06 | 2014-12-03 | 南昌大学 | Method for comprehensively extracting tea seed saponin, tea seed polypeptide and tea seed polysaccharide from tea seed cake |
| CN104212647A (en) * | 2014-09-11 | 2014-12-17 | 陈育烨 | Preparation method of pure natural tea seed detergent |
| CN104479889A (en) * | 2014-11-15 | 2015-04-01 | 陈育烨 | Preparation method of tea seed cleanser |
| CN107312618A (en) * | 2017-07-31 | 2017-11-03 | 湖南楚宏生物科技有限公司 | A kind of tea oil high-efficiency purifying method |
| CN108486715A (en) * | 2018-05-03 | 2018-09-04 | 广东护康宝农林生物科技有限公司 | A kind of Tea Saponin washes clean bag and its application method |
| CN108522550A (en) * | 2018-04-28 | 2018-09-14 | 浦江县欧立生物技术有限公司 | A kind of preparation method of sterilizing synergistic agent |
| CN110437299A (en) * | 2019-07-09 | 2019-11-12 | 合肥学院 | A kind of extracting method of Tea Saponin |
| CN110759447A (en) * | 2019-11-24 | 2020-02-07 | 南京山禾生态环境有限公司 | Modified attapulgite powder for removing algae by coagulation |
| CN111449090A (en) * | 2020-04-13 | 2020-07-28 | 湖南润农生态茶油有限公司 | Preparation method of tea seed cake extract |
| CN111939210A (en) * | 2019-05-17 | 2020-11-17 | 赣南医学院 | Tea seed cake extract and application thereof |
| CN112047994A (en) * | 2020-07-13 | 2020-12-08 | 安徽裕民生态农业有限公司 | Method for extracting tea saponin from camellia seed meal |
-
2009
- 2009-03-14 CN CN200910021714A patent/CN101817853A/en active Pending
Cited By (23)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101967177A (en) * | 2010-09-17 | 2011-02-09 | 华中农业大学 | Extract and method for extracting tea saponin from oil-tea seed residue |
| CN102028042A (en) * | 2010-10-28 | 2011-04-27 | 福建省尤溪县沈郎食用油有限公司 | Method and equipment for preparing tea seed oil from tea seeds and extracting tea polyphenol from byproduct tea seed cake |
| CN102028042B (en) * | 2010-10-28 | 2013-01-02 | 福建省尤溪县沈郎食用油有限公司 | Method and equipment for preparing tea seed oil from tea seeds and extracting tea polyphenol from byproduct tea seed cake |
| CN102020692A (en) * | 2010-12-15 | 2011-04-20 | 华中科技大学 | Method for extracting refined tea saponin from camellia oleifera seed cake |
| CN102020692B (en) * | 2010-12-15 | 2012-09-26 | 华中科技大学 | Method for extracting refined tea saponin from camellia oleifera seed cake |
| CN102659902A (en) * | 2012-05-02 | 2012-09-12 | 湖南山润油茶科技发展有限公司 | Process for extracting high-purity tea saponin from tea seed cakes |
| CN102659902B (en) * | 2012-05-02 | 2014-07-23 | 湖南山润油茶科技发展有限公司 | Process for extracting high-purity tea saponin from tea seed cakes |
| CN103509069A (en) * | 2012-06-27 | 2014-01-15 | 上海莱博生物科技有限公司 | Preparation method of crude product of tea saponin and preparation method of tea saponin B1 |
| CN103950639A (en) * | 2014-05-20 | 2014-07-30 | 贵州大学 | Method of storing tea seed pancake by utilizing vacuum package |
| CN104177508B (en) * | 2014-08-06 | 2016-05-11 | 南昌大学 | The comprehensive method of extracting thea saponin, tea seed polypeptide, tea seed polysaccharide in leached tea oil slag |
| CN104177508A (en) * | 2014-08-06 | 2014-12-03 | 南昌大学 | Method for comprehensively extracting tea seed saponin, tea seed polypeptide and tea seed polysaccharide from tea seed cake |
| CN104212647A (en) * | 2014-09-11 | 2014-12-17 | 陈育烨 | Preparation method of pure natural tea seed detergent |
| CN104479889A (en) * | 2014-11-15 | 2015-04-01 | 陈育烨 | Preparation method of tea seed cleanser |
| CN107312618A (en) * | 2017-07-31 | 2017-11-03 | 湖南楚宏生物科技有限公司 | A kind of tea oil high-efficiency purifying method |
| CN108522550A (en) * | 2018-04-28 | 2018-09-14 | 浦江县欧立生物技术有限公司 | A kind of preparation method of sterilizing synergistic agent |
| CN108486715A (en) * | 2018-05-03 | 2018-09-04 | 广东护康宝农林生物科技有限公司 | A kind of Tea Saponin washes clean bag and its application method |
| CN108486715B (en) * | 2018-05-03 | 2019-04-26 | 广东护康宝农林生物科技有限公司 | A kind of Tea Saponin washes clean bag and its application method |
| CN111939210A (en) * | 2019-05-17 | 2020-11-17 | 赣南医学院 | Tea seed cake extract and application thereof |
| CN110437299A (en) * | 2019-07-09 | 2019-11-12 | 合肥学院 | A kind of extracting method of Tea Saponin |
| CN110437299B (en) * | 2019-07-09 | 2020-09-18 | 合肥学院 | Extraction method of tea saponin |
| CN110759447A (en) * | 2019-11-24 | 2020-02-07 | 南京山禾生态环境有限公司 | Modified attapulgite powder for removing algae by coagulation |
| CN111449090A (en) * | 2020-04-13 | 2020-07-28 | 湖南润农生态茶油有限公司 | Preparation method of tea seed cake extract |
| CN112047994A (en) * | 2020-07-13 | 2020-12-08 | 安徽裕民生态农业有限公司 | Method for extracting tea saponin from camellia seed meal |
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Application publication date: 20100901 |