CN104961793A - Method for extracting high-purity tea saponin from tea seed cake dregs - Google Patents
Method for extracting high-purity tea saponin from tea seed cake dregs Download PDFInfo
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- CN104961793A CN104961793A CN201510366998.1A CN201510366998A CN104961793A CN 104961793 A CN104961793 A CN 104961793A CN 201510366998 A CN201510366998 A CN 201510366998A CN 104961793 A CN104961793 A CN 104961793A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07J—STEROIDS
- C07J63/00—Steroids in which the cyclopenta(a)hydrophenanthrene skeleton has been modified by expansion of only one ring by one or two atoms
- C07J63/008—Expansion of ring D by one atom, e.g. D homo steroids
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H15/00—Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
- C07H15/20—Carbocyclic rings
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Abstract
The invention discloses a method for extracting high-purity tea saponin from tea seed cake dregs. The method comprises the following steps that the tea seed cake dregs are smashed, then ethyl alcohol with the weight ratio of 1:4-7 is added to the tea seed cake dregs to be stirred in an ultrasonic stirrer for 20-30 min, and mixed liquor is obtained; the mixed liquor is transferred to a return device for return extraction, and an extracting solution is obtained; the pH value of the extracting solution is adjusted to three to four through citric acid for vacuum concentration, and a tea saponin crude product is obtained through drying; silica-gel column chromatography is carried out on the crude product, and a dried solid is dissolved with methyl alcohol, and is recrystallized, filtered and dried, and the high-purity tea saponin can be obtained. The extracting rate of the tea saponin is 50 percent to 57 percent, purity is over 98.0 percent, the extracting method has the advantages of being easy to operate, short in time, high in extraction rate, high in purity and low in cost, achieving low-energy-consumption extraction and the like, and industrial production can be achieved easily.
Description
Technical field
The present invention relates to technical field of agricultural product process, especially a kind of method extracting high-purity tea saponin from cake of camellia oleifera seeds.
Background technology
Tea tree oil meal is also known as tea cake, oil cake, the tea dregs of rice, and be residuum after tea seed oil expression, annual tea seed output, at about 650,000 t, about produces the tea waste of 150,000 t tea oil and 500,000 t.Current mainly concentrate on tea saponin to the research of biologically active substance in tea tree oil meal both at home and abroad, the content of tea saponin in tea tree oil meal is 10 ~ 20%.Tea saponin has another name called TS, is that its molecular formula is: C by the class candy glucoside compound extracted in tea tree seed
57h
90o
26, basic carbon skeleton belongs to pentacyclic triterpenoid for neat honest fruit alkane, is made up of aglycon, sugared body and organic acid three part.The physico-chemical property of tea saponin is that tea saponin sterling is creamy white or pale yellow powder, and the tea saponin containing impurity is generally in brown, and the higher color of purity is more shallow.Its polarity is comparatively large, is generally dissolved in the larger solvent of polarity, is dissolved in methyl alcohol, ethanol, butanols, amylalcohol etc., is insoluble to ether, chloroform, sherwood oil equal solvent.
Tea saponin is a kind of excellent natural nonionic surface active agent, has the pharmacological function such as the surface-active actions such as emulsification, dispersion, moistening, foaming and impervious, anti-inflammatory, analgesia.Current tea saponin has been widely used in fields such as foodstuffs industry, makeup, construction industry, medicine and agricultural chemicals, and existing report tea saponin prepares the products such as senior nuisanceless washing composition, sanitising agent, foaming agent, emulsifying agent, sterilant, shampoo at present.
The multiple method of scientists extracts tea saponin from tea waste, the technique extracting tea saponin as water extraction is: tea seed cake-pulverizing-hot-water soak-filtration-concentrated-decolouring-reconcentration-decolour-tea saponin again, though the method extraction process is comparatively simple, the tea saponin purity that the method is extracted is very low, yield also reduces.The technical process that organic solvent method extracts tea saponin is: tea seed cake-pulverizing-thick saponin of sherwood oil backflow degrease-alcohol reflux-filtration-concentrated-acetone precipitation-vacuum-drying one, the product purity that the method is extracted and yield are improved, but extraction process is complicated, cost is high, power consumption is large, extraction process is longer.In recent years, also scientist is had to do further improvement to water extraction and organic solvent method extraction process, but at present the extraction process of tea saponin also exist purity and yield be not very desirable, extraction process is complicated, power consumption is large, cost is high, have the problems such as larger pollution, be difficult to realize suitability for industrialized production.
Summary of the invention
The deficiency that extraction process for existing tea saponin exists by the present invention, provides a kind of method extracting high-purity tea saponin from tea waste.The method is extracted the tea saponin purity obtained and is reached more than 98%, and yield there has also been larger raising, and the method operating procedure is simple, cost is low, be easy to realize suitability for industrialized production.
In order to realize above object, the technical solution used in the present invention is:
From tea waste, extract a method for high-purity tea saponin, comprise the following steps:
(1) tea waste is pulverized, obtain tea waste powder;
(2) add in ultrasonic stirrer by tea waste powder, adding with its weight ratio is the ethanol of 1:4-7, then stirs 20-30min, obtains mixed solution;
(3) again mixed solution is transferred to reflux, refluxing extraction 3-4 time, reflux 0.5-1h at every turn, united extraction liquid;
(4) by said extracted liquid temperature be 50-60 DEG C, pressure be the condition of 0.05-0.08Mpa under concentrating under reduced pressure 2-3h, concentrated solution can be obtained, the pH value 3-4 of concentrated solution is regulated again with citric acid, by throw out after filtering, be dry 1-2h under the condition of 50-60 DEG C in temperature, tea saponin crude product can be obtained;
(5) after tea saponin crude product dissolve with methanol through filtering, the filtrate obtained, through silica gel column chromatography, is made into elutriant with methyl alcohol and the water that volume ratio is 3:1, finally collects sample solution after wash-out, by sample solution drying at 50-60 DEG C, obtains solids;
(6) dissolved by solids with methyl alcohol again, then use ordinary method recrystallization, filter, the crystallisate obtained is dry at 50-60 DEG C, can obtain high-purity tea saponin.
A kind of the above method extracting high-purity tea saponin from tea waste, described pulverizing is that tea waste is crushed to 60-80 order.
A kind of the above method extracting high-purity tea saponin from tea waste, the alcohol concn described in step (2) is 85-95%.
A kind of the above method extracting high-purity tea saponin from tea waste, the stirring velocity of step (2) is 300-800r/min.
A kind of the above method extracting high-purity tea saponin from tea waste, described citric acid concentration is 5-10%.
A kind of the above method extracting high-purity tea saponin from tea waste, the concentration of described methyl alcohol is 90-95%.
A kind of the above method extracting high-purity tea saponin from tea waste, the purity of described high-purity tea saponin reaches more than 98%.
Compared with prior art, the beneficial effect that the present invention obtains is:
(1) in the present invention before refluxing extraction tea saponin first through ultrasonic stirring, utilizing hyperacoustic cavatition to make, tea saponin is easier extracts from tea waste, after ultrasonic wave makes extracting solution constantly be shaken simultaneously, more be conducive to solutes accumulation, thus further improve the extraction yield of tea saponin.
(2) before refluxing extraction tea saponin of the present invention first through ultrasonic stirring, shorten the return time of half.
(3) in the present invention, tea saponin extraction yield and purity are all very high, and wherein extraction rate reached is to 50-57%, and purity reaches more than 98.0%, reach the requirement of standard substance.
(4) extracting method of the present invention also have simple to operate, consume energy low, the time is short, low cost and other advantages, be easy to realize suitability for industrialized production.
Embodiment
Below in conjunction with specific embodiment, the present invention is further described, but be not limited to protection scope of the present invention.
embodiment 1
From tea waste, extract a method for high-purity tea saponin, comprise the following steps:
(1) 5kg tea waste (wherein the content of tea saponin is 0.9kg) is crushed to 60 orders, obtains tea waste powder;
(2) above-mentioned tea waste powder is added in ultrasonic stirrer, then add the ethanol 20L that concentration is 90%, start agitator, under rotating speed is 300r/min, stirs 20min, obtains mixed solution;
(3) again mixed solution is transferred to reflux, refluxing extraction 3 times, reflux 0.5h at every turn, united extraction liquid;
(4) by said extracted liquid temperature be 60 DEG C, pressure be the condition of 0.07Mpa under concentrating under reduced pressure 2h, concentrated solution can be obtained, the pH value 3 of concentrated solution is regulated again with the citric acid that concentration is 5%, by throw out after filtering, be dry 2h under the condition of 50 DEG C in temperature, tea saponin crude product can be obtained;
(5) tea saponin crude product 1L concentration is the dissolve with methanol of 90%, more after filtration, the filtrate obtained is through silica gel column chromatography, be that the methyl alcohol of 3:1 and water are made into elutriant by volume ratio, finally sample solution is collected after wash-out, sample solution is dry at 60 DEG C, obtain solids;
(6) dissolved by solids with the methyl alcohol that concentration is 90% again, then use ordinary method recrystallization, filter, the crystallisate obtained is dry at 60 DEG C, can obtain 0.458 kg high-purity tea saponin.
In the present embodiment, the extraction yield (extraction yield of tea saponin is the content of tea saponin in tea waste and the mass percent of the high-purity tea saponin obtained) of tea saponin reaches 50.89%, and purity is 98.21%.
embodiment 2
From tea waste, extract a method for high-purity tea saponin, comprise the following steps:
(1) 5kg tea waste (wherein the content of tea saponin is 0.9kg) is crushed to 80 orders, obtains tea waste powder;
(2) above-mentioned tea waste powder is added in ultrasonic stirrer, then add the ethanol 25L that concentration is 95%, start agitator, under rotating speed is 500r/min, stirs 25min, obtains mixed solution;
(3) again mixed solution is transferred to reflux, refluxing extraction 3 times, reflux 40min at every turn, united extraction liquid;
(4) by said extracted liquid temperature be 50 DEG C, pressure be the condition of 0.06Mpa under concentrating under reduced pressure 3h, concentrated solution can be obtained, the pH value 4 of concentrated solution is regulated again with the citric acid that concentration is 5%, by throw out after filtering, be dry 1h under the condition of 60 DEG C in temperature, tea saponin crude product can be obtained;
(5) tea saponin crude product 1L concentration is the dissolve with methanol of 90%, more after filtration, the filtrate obtained is through silica gel column chromatography, be that the methyl alcohol of 3:1 and water are made into elutriant by volume ratio, finally sample solution is collected after wash-out, sample solution is dry at 60 DEG C, obtain solids;
(6) dissolved by solids with the methyl alcohol that concentration is 90% again, then use ordinary method recrystallization, filter, the crystallisate obtained is dry at 60 DEG C, can obtain 0.475kg high-purity tea saponin.
In the present embodiment, the extraction yield (extraction yield of tea saponin is the content of tea saponin in tea waste and the mass percent of the high-purity tea saponin obtained) of tea saponin reaches 52.78%, and purity is 98.11%.
embodiment 3
From tea waste, extract a method for high-purity tea saponin, comprise the following steps:
(1) 5kg tea waste (wherein the content of tea saponin is 0.9kg) is crushed to 60 orders, obtains tea waste powder;
(2) above-mentioned tea waste powder is added in ultrasonic stirrer, then add the ethanol 35L that concentration is 90%, start agitator, under rotating speed is 500r/min, stirs 30min, obtains mixed solution;
(3) again mixed solution is transferred to reflux, refluxing extraction 3 times, reflux 1h at every turn, united extraction liquid;
(4) by said extracted liquid temperature be 60 DEG C, pressure be the condition of 0.08Mpa under concentrating under reduced pressure 2h, concentrated solution can be obtained, the pH value 3 of concentrated solution is regulated again with the citric acid that concentration is 8%, by throw out after filtering, be dry 2h under the condition of 60 DEG C in temperature, tea saponin crude product can be obtained;
(5) tea saponin crude product 1L concentration is the dissolve with methanol of 95%, more after filtration, the filtrate obtained is through silica gel column chromatography, be that the methyl alcohol of 3:1 and water are made into elutriant by volume ratio, finally sample solution is collected after wash-out, sample solution is dry at 60 DEG C, obtain solids;
(6) dissolved by solids with the methyl alcohol of 95% again, then use ordinary method recrystallization, filter, the crystallisate obtained is dry at 60 DEG C, can obtain 0.506 kg high-purity tea saponin.
In the present embodiment, the extraction yield (extraction yield of tea saponin is the content of tea saponin in tea waste and the mass percent of the high-purity tea saponin obtained) of tea saponin reaches 56.22%, and purity is 98.57%.
embodiment 4
From tea waste, extract a method for high-purity tea saponin, comprise the following steps:
(1) 5kg tea waste (wherein the content of tea saponin is 0.9kg) is crushed to 60 orders, obtains tea waste powder;
(2) above-mentioned tea waste powder is added in ultrasonic stirrer, then add the ethanol 30L that concentration is 85%, start agitator, under rotating speed is 300r/min, stirs 30min, obtains mixed solution;
(3) again mixed solution is transferred to reflux, refluxing extraction 3 times, reflux 1h at every turn, united extraction liquid;
(4) by said extracted liquid temperature be 50 DEG C, pressure be the condition of 0.07Mpa under concentrating under reduced pressure 3h, concentrated solution can be obtained, the pH value 4 of concentrated solution is regulated again with the citric acid that concentration is 10%, by throw out after filtering, be dry 2h under the condition of 50 DEG C in temperature, tea saponin crude product can be obtained;
(5) tea saponin crude product 1L concentration is the dissolve with methanol of 95%, more after filtration, the filtrate obtained is through silica gel column chromatography, be that the methyl alcohol of 3:1 and water are made into elutriant by volume ratio, finally sample solution is collected after wash-out, sample solution is dry at 60 DEG C, obtain solids;
(6) dissolved by solids with the methyl alcohol of 95% again, then use ordinary method recrystallization, filter, the crystallisate obtained is dry at 60 DEG C, can obtain 0.462 kg high-purity tea saponin.
In the present embodiment, the extraction yield (extraction yield of tea saponin is the content of tea saponin in tea waste and the mass percent of the high-purity tea saponin obtained) of tea saponin reaches 51.28%, and purity is 98.18%.
Claims (7)
1. from tea waste, extract a method for high-purity tea saponin, it is characterized in that, comprise the following steps:
(1) tea waste is pulverized, obtain tea waste powder;
(2) add in ultrasonic stirrer by tea waste powder, adding with its weight ratio is the ethanol of 1:4-7, then stirs 20-30min, obtains mixed solution;
(3) again mixed solution is transferred to reflux, refluxing extraction 3-4 time, reflux 0.5-1h at every turn, united extraction liquid;
(4) by said extracted liquid temperature be 50-60 DEG C, pressure be the condition of 0.05-0.08Mpa under concentrating under reduced pressure 2-3h, concentrated solution can be obtained, the pH value 3-4 of concentrated solution is regulated again with citric acid, by throw out after filtering, be dry 1-2h under the condition of 50-60 DEG C in temperature, tea saponin crude product can be obtained;
(5) after tea saponin crude product dissolve with methanol through filtering, the filtrate obtained, through silica gel column chromatography, is made into elutriant with methyl alcohol and the water that volume ratio is 3:1, finally collects sample solution after wash-out, by sample solution drying at 50-60 DEG C, obtains solids;
(6) dissolved by solids with methyl alcohol again, then use ordinary method recrystallization, filter, the crystallisate obtained is dry at 50-60 DEG C, can obtain high-purity tea saponin.
2. a kind of method extracting high-purity tea saponin from tea waste according to claim 1, is characterized in that: described pulverizing is that tea waste is crushed to 60-80 order.
3. a kind of method extracting high-purity tea saponin from tea waste according to claim 1, is characterized in that: the alcohol concn described in step (2) is 85-95%.
4. a kind of method extracting high-purity tea saponin from tea waste according to claim 1, is characterized in that: the stirring velocity of step (2) is 300-800r/min.
5. a kind of method extracting high-purity tea saponin from tea waste according to claim 4, is characterized in that: described citric acid concentration is 5-10%.
6. a kind of method extracting high-purity tea saponin from tea waste according to claim 5, is characterized in that: the concentration of described methyl alcohol is 90-95%.
7. a kind of method extracting high-purity tea saponin from tea waste according to claim 6, is characterized in that: the purity of described high-purity tea saponin reaches more than 98%.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106967144A (en) * | 2017-03-28 | 2017-07-21 | 钦州市桂耘贸易有限公司 | A kind of method that Tea Saponin is extracted from tea bran |
| CN107496275A (en) * | 2017-10-18 | 2017-12-22 | 湖南大三湘茶油电子商务有限公司 | Camellia seed washes clean stoste and preparation method thereof |
| CN107496308A (en) * | 2017-10-18 | 2017-12-22 | 湖南大三湘茶油电子商务有限公司 | Facial mask stoste and preparation method thereof is nourished in the reparation of camellia anti-acne |
| CN107653055A (en) * | 2017-09-29 | 2018-02-02 | 浙江工业大学 | A kind of method of ultrasonic wave added extracting tea seed oil by using enzymatic hydrolysis |
| CN108948124A (en) * | 2018-08-01 | 2018-12-07 | 永兴县悠香山茶油有限公司 | A kind of preparation method of Tea Saponin |
| CN113307840A (en) * | 2021-05-20 | 2021-08-27 | 湖南万象生物科技有限公司 | High-purity tea saponin prepared by water method and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107653055A (en) * | 2017-09-29 | 2018-02-02 | 浙江工业大学 | A kind of method of ultrasonic wave added extracting tea seed oil by using enzymatic hydrolysis |
| CN107496275A (en) * | 2017-10-18 | 2017-12-22 | 湖南大三湘茶油电子商务有限公司 | Camellia seed washes clean stoste and preparation method thereof |
| CN107496308A (en) * | 2017-10-18 | 2017-12-22 | 湖南大三湘茶油电子商务有限公司 | Facial mask stoste and preparation method thereof is nourished in the reparation of camellia anti-acne |
| CN108948124A (en) * | 2018-08-01 | 2018-12-07 | 永兴县悠香山茶油有限公司 | A kind of preparation method of Tea Saponin |
| CN113307840A (en) * | 2021-05-20 | 2021-08-27 | 湖南万象生物科技有限公司 | High-purity tea saponin prepared by water method and preparation method thereof |
| CN113307840B (en) * | 2021-05-20 | 2022-05-27 | 湖南万象生物科技有限公司 | High-purity tea saponin prepared by water method and preparation method thereof |
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Application publication date: 20151007 |