CN112225774A - Novel method for extracting tea saponin with high purity and high extraction rate - Google Patents
Novel method for extracting tea saponin with high purity and high extraction rate Download PDFInfo
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- CN112225774A CN112225774A CN201910581927.1A CN201910581927A CN112225774A CN 112225774 A CN112225774 A CN 112225774A CN 201910581927 A CN201910581927 A CN 201910581927A CN 112225774 A CN112225774 A CN 112225774A
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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
- C07H15/24—Condensed ring systems having three or more rings
- C07H15/256—Polyterpene radicals
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Abstract
The invention provides a novel method for extracting tea saponin with high purity and high extraction rate, which comprises the following steps: (1) drying and crushing the camellia seed meal, mixing grinding aids, and carrying out solid-state grinding; (2) adding water into the mixture obtained in the step 1), stirring, extracting and filtering to obtain filtrate; (3) adding acid to obtain a crystalline tea saponin crude product; (4) adding the aqueous ethanol-acetone composite solvent into the crude product of the tea saponin, and stirring; (5) adding sterol complexing agent into the obtained mixture for complexing treatment; (6) and carrying out decomplexing separation treatment on the mixture to obtain the high-purity tea saponin. (7) Separating and recovering the solvent, filtering or centrifugally separating the leaching solution, and simultaneously decompressing and evaporating to recover the organic solvent in the leaching solution to obtain a tea saponin aqueous solution; then removing water to obtain a tea saponin mixture; (8) and (4) decoloring and spray-drying the tea saponin solution in the step (7) to obtain the high-purity tea saponin. Compared with the prior art, the method overcomes the defect of low extraction rate of the tea saponin by the existing organic solvent extraction method, the purity of the tea saponin obtained by the provided extraction method is up to more than 98%, the process is simple and convenient, the cost is low, the tea saponin can be efficiently purified, and the method is suitable for large-scale production.
Description
Technical Field
The invention relates to the field of extraction of tea saponin in an organic chemical technology, discloses a method for extracting tea saponin by utilizing a biotechnology, and particularly relates to a novel method for extracting tea saponin with high purity and high extraction rate.
Background
The tea saponin is also called tea saponin, is a pentacyclic three-part material, has hydrophilic saccharide and hydrophobic sapogenin, is a natural nonionic surfactant with good performance, has surface active effects of emulsification, dispersion, wetting, foaming and the like, has pharmacological functions of permeability resistance, inflammation resistance, pain relief and the like, can also sterilize, kill insects and powerfully decontaminate, and can be widely applied to the fields of light industry, chemical industry, pesticides, feeds, cultivation, textiles and the like. Tea saponin has good water solubility, abundant foam and strong detergency, is an excellent material for the washing product industry and the emulsifier industry, is a glycoside compound, is mainly extracted from tea plant species as the name suggests, and tea resources in China are very abundant, wherein the area of a tea-oil tree forest is about 5500 ten thousand mu, and production raw materials are easy to obtain, so the cost is low, and tea seed meal obtained by primary treatment contains a large amount of tea saponin and other useful substances and has a thick potential added value.
At present, the extraction method of tea saponin mainly comprises four major methods, namely a water immersion method, an organic solvent extraction method, an adsorption extraction method and a combined immersion method of an organic solvent and water. The water immersion method mainly comprises extracting tea saponin with water containing inorganic acid as solvent, and treating the extractive solution with precipitation, flocculation, and clarifying agent such as aluminum salt to remove main impurities. The organic solvent extraction method mainly uses water-containing methanol, water-containing ethanol, water-containing propanol and the like to extract raw materials, and utilizes the solubility difference of tea saponin and impurities in different organic solvents to extract high-purity tea saponin from the raw materials. The adsorption extraction method is that the tea saponin in the solution is adsorbed by the multi-purpose adsorbent, and impurities are separated and purified. The combination method uses water as medium in the leaching stage, uses organic solvent for purification, and uses neutral water as medium. However, the methods have technical problems, and the tea seed meal raw material in the water immersion method has more impurities and is difficult to filter; the organic solvent extraction method has the advantages of more extraction times, long working procedure time and high time cost; the adsorption method and the combination method also utilize the solubility difference of the tea saponin, protein and other impurities in different solvents, and have low extraction rate, high cost and low cost performance.
Disclosure of Invention
The invention aims to provide a novel method for extracting tea saponin with high purity and high extraction rate, and the purity and the extraction rate of the tea saponin obtained by the method are higher than those of the conventional extraction method. The invention provides novel tea saponin with high purity and high extraction rate, which comprises the following steps.
(1) Drying and crushing the camellia seed meal, mixing grinding aids, and carrying out solid-state grinding;
(2) adding water into the mixture obtained in the step (1), stirring, extracting and filtering to obtain filtrate;
(3) adding acid into the filtrate obtained in the step (2) to obtain a crystalline tea saponin crude product;
(4) adding the aqueous ethanol-acetone composite solvent into the crude product of the tea saponin, and stirring;
(5) adding sterol complexing agent into the obtained mixture for complexing treatment;
(6) carrying out decomplexing separation treatment on the mixture obtained in the step (5) to obtain high-purity tea saponin;
(7) separating and recovering the solvent, filtering or centrifugally separating the leaching solution, and simultaneously decompressing and evaporating to recover the organic solvent in the leaching solution to obtain a tea saponin aqueous solution; then removing water to obtain a tea saponin mixture;
(8) decoloring and spray-drying the tea saponin solution in the step (7) to obtain high-purity tea saponin;
the further preferred scheme of the invention is that the tea saponin is directly extracted by taking the camellia seeds as the raw material, and the drying temperature of the camellia seeds is 80 ℃;
the further preferable scheme of the invention is that the proportion of the grinding aid to the rapeseed dregs is 1:50, and the grinding time is 4 h;
the further preferable scheme of the invention is that the ratio of the acid addition amount to the filtrate is 1: 90, stirring for 12 hours;
the further preferable scheme of the invention is that the proportion of the hydrous ethanol-acetone composite solvent to the total amount of the mixture is 1:85, and the proportion of the sterol complexing agent to the total amount of the mixture is 1: 37;
in a further preferred embodiment of the present invention, the sterol complexing agent is cholesterol, sitosterol, or legumesterol
The further preferable scheme of the invention is that the precipitated crystal is washed for 2-3 times by absolute ethyl alcohol, and then is vaporized and dehydrated, and the heating temperature is 60-120 ℃, and the time is 4-6 h;
the invention further preferably adopts the scheme that sterol complexing agents are added into the tea saponin extracting solution, and the mixture is sequentially heated, concentrated and filtered to obtain the tea saponin complex.
Detailed Description
The technical solution of the present patent will be described in further detail with reference to the following embodiments.
The invention provides a method for extracting tea saponin, which comprises the following steps:
(1) drying and crushing the camellia seed meal, mixing grinding aids, and carrying out solid-state grinding;
(2) adding water into the mixture obtained in the step (1), stirring, extracting and filtering to obtain filtrate;
(3) adding acid into the filtrate obtained in the step (2) to obtain a crystalline tea saponin crude product;
(4) adding the aqueous ethanol-acetone composite solvent into the crude product of the tea saponin, and stirring;
(5) adding sterol complexing agent into the obtained mixture for complexing treatment;
(6) carrying out decomplexing separation treatment on the mixture obtained in the step (5) to obtain high-purity tea saponin;
(7) separating and recovering the solvent, filtering or centrifugally separating the leaching solution, and simultaneously decompressing and evaporating to recover the organic solvent in the leaching solution to obtain a tea saponin aqueous solution; then removing water to obtain a tea saponin mixture;
(8) and (4) decoloring and spray-drying the tea saponin solution in the step (7) to obtain the high-purity tea saponin.
The following examples are given for the purpose of illustration.
Examples
(1) Drying and crushing 500g of camellia seed meal, mixing 50g of grinding aid, and carrying out solid-state grinding;
(2) adding 1000ml of water into the mixture obtained in the step (1), stirring, extracting and filtering to obtain filtrate; stirring at 120 deg.C for 1.5 h;
(3) adding 100ml of organic acid into the filtrate obtained in the step (2) to obtain a crystalline tea saponin crude product;
(4) heating the crystal at 160 deg.C for 1.5h, adding 25ml of aqueous ethanol-acetone composite solvent, and stirring for 2 h;
(5) adding 28g of sterol complexing agent into the obtained mixture for complexing treatment; vacuum concentrating at low temperature for 3 hr, and vacuum filtering and drying to obtain tea saponin complex;
(6) carrying out decomplexing separation treatment on the mixture obtained in the step (5), and carrying out hot filtration to obtain high-purity tea saponin;
(7) separating and recovering the solvent, filtering or centrifugally separating the leaching solution, and simultaneously decompressing and evaporating to recover the organic solvent in the leaching solution to obtain a tea saponin aqueous solution; then removing water for 1h to obtain a tea saponin mixture;
(8) and (4) decoloring and spray-drying the tea saponin solution in the step (7) to obtain the high-purity tea saponin.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention, and it is not intended to limit the present invention to the embodiments shown herein, and modifications and variations can be made thereto by those skilled in the art without departing from the scope of the invention as defined in the appended claims.
Claims (7)
1. The novel method for extracting the tea saponin with high purity and high extraction rate is characterized by comprising the following steps:
(1) drying and crushing the camellia seed meal, mixing grinding aids, and carrying out solid-state grinding;
(2) adding water into the mixture obtained in the step (1), stirring, extracting and filtering to obtain filtrate;
(3) adding acid into the filtrate obtained in the step (2) to obtain a crystalline tea saponin crude product;
(4) adding the aqueous ethanol-acetone composite solvent into the crude product of the tea saponin, and stirring;
(5) adding sterol complexing agent into the obtained mixture for complexing treatment;
(6) carrying out decomplexing separation treatment on the mixture obtained in the step (5) to obtain high-purity tea saponin;
(7) separating and recovering the solvent, filtering or centrifugally separating the leaching solution, and simultaneously decompressing and evaporating to recover the organic solvent in the leaching solution to obtain a tea saponin aqueous solution; then removing water to obtain a tea saponin mixture;
(8) and (4) decoloring and spray-drying the tea saponin solution in the step (7) to obtain the high-purity tea saponin.
2. The method for extracting tea saponin with high purity and high extraction rate as claimed in claim 1, wherein the tea saponin is extracted directly from the seeds of Camellia oleifera Abel at 80 deg.C.
3. The method for extracting theasaponin with high purity and high extraction rate as claimed in claim 1, wherein the ratio of grinding aid to rapeseed meal is 1:50, and the grinding time is 4 h.
4. The method for extracting theasaponin with high purity and high extraction rate as claimed in claim 1, wherein: the proportion of acid addition and filtrate is 1: 90, the stirring time is 12 h.
5. The method for extracting theasaponin with high purity and high extraction rate as claimed in claim 1, wherein: the ratio of the aqueous ethanol-acetone composite solvent to the total amount of the mixture is 1:85, and the ratio of the sterol complexing agent to the total amount of the mixture is 1: 37.
6. The method for extracting theasaponin with high purity and high extraction rate as claimed in claim 1, wherein: washing the precipitated crystal with absolute ethyl alcohol for 2-3 times, then evaporating and dehydrating, and heating for 4-6 h at the temperature of 60-120 ℃.
7. The method for extracting theasaponin with high purity and high extraction rate as claimed in claim 1, wherein: leaching is repeated for 1-2 times before filtering or centrifuging.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201910581927.1A CN112225774A (en) | 2019-06-30 | 2019-06-30 | Novel method for extracting tea saponin with high purity and high extraction rate |
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| CN201910581927.1A CN112225774A (en) | 2019-06-30 | 2019-06-30 | Novel method for extracting tea saponin with high purity and high extraction rate |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113018896A (en) * | 2021-03-03 | 2021-06-25 | 北京林业大学 | Natural saponin decoloring method |
| CN113061155A (en) * | 2021-03-18 | 2021-07-02 | 广州妙思生物科技有限公司 | Method for extracting tea saponin from camellia seeds |
| CN113264980A (en) * | 2021-05-20 | 2021-08-17 | 湖南万象生物科技有限公司 | High-purity tea seed meal protein and tea saponin and preparation method thereof |
-
2019
- 2019-06-30 CN CN201910581927.1A patent/CN112225774A/en not_active Withdrawn
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113018896A (en) * | 2021-03-03 | 2021-06-25 | 北京林业大学 | Natural saponin decoloring method |
| CN113018896B (en) * | 2021-03-03 | 2022-08-26 | 北京林业大学 | Natural saponin decoloring method |
| CN113061155A (en) * | 2021-03-18 | 2021-07-02 | 广州妙思生物科技有限公司 | Method for extracting tea saponin from camellia seeds |
| CN113264980A (en) * | 2021-05-20 | 2021-08-17 | 湖南万象生物科技有限公司 | High-purity tea seed meal protein and tea saponin and preparation method thereof |
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