CN111018940A - Method for extracting oil saponin from oil-tea camellia cakes - Google Patents
Method for extracting oil saponin from oil-tea camellia cakes Download PDFInfo
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- CN111018940A CN111018940A CN201911386994.4A CN201911386994A CN111018940A CN 111018940 A CN111018940 A CN 111018940A CN 201911386994 A CN201911386994 A CN 201911386994A CN 111018940 A CN111018940 A CN 111018940A
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- saponin
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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 relates to a preparation method of oil saponin, in particular to a method for extracting oil saponin from a camellia oleifera cake. A method for extracting oil saponin from oil tea cakes comprises the following steps: 1) crushing the oil tea cake serving as a raw material, adding a solvent, heating and extracting for 1-2 times, filtering, and collecting an extracting solution; the solvent is a sodium hydroxide aqueous solution, a sodium carbonate aqueous solution, a sodium bicarbonate aqueous solution or a potassium carbonate aqueous solution with the pH value of 11-14; 2) adjusting the pH of the extracting solution to be less than or equal to 2 by using acid, stirring, standing, performing suction filtration, and collecting a filter cake; 3) dissolving the filter cake with water, passing through a macroporous resin column, washing the resin column with water until effluent liquid is colorless, eluting with ethanol or methanol with volume concentration of 60-80%, tracking and detecting by thin layer chromatography, and collecting alcohol eluent; the model of the macroporous resin is D-900, ADS-7 or LSA-700; 4) concentrating the eluate, adding a small amount of high-purity tea saponin into the concentrated solution, standing for crystallization, separating out crystals, and drying to obtain high-purity tea saponin.
Description
Technical Field
The invention relates to a preparation method of oil saponin, in particular to a method for extracting oil saponin from a camellia oleifera cake.
Background
The Camellia oleifera Abel is cake-like residue obtained by pressing kernel of Camellia oleifera Abel (Camellia oleifera Abel) belonging to Camellia genus and evergreen small arbor of Theaceae family. The oil tea cake contains fat, protein, crude fiber, tea saponin, saccharide and a small amount of polyphenol antioxidant active substances, and can extract residual oil, tea saponin, polyphenol and other substances from the oil tea cake, wherein the content of the tea saponin in the oil tea cake is up to 15%. The tea saponin is also called tea saponin, belongs to triterpenoid saponin, has bitter, pungent and pungent taste, stimulates nasal mucosa to cause sneezing, is a white fine columnar crystal in a pure product, and has strong hygroscopicity; the natural glycoside compound surfactant has good performance, can be widely applied to the fields of light industry, chemical industry, pesticides, feed, cultivation, spinning, oil extraction, mining, building materials, highway construction and the like, and has higher economic value.
The invention discloses a method for extracting and refining tea saponin, which is disclosed by the invention with the publication number of CN1148598, and is characterized in that a tea-oil cake is taken as a raw material, domestic styrene type copolymer resin is adopted to adsorb the tea saponin in a tea-oil cake leaching solution, an organic or inorganic alkaline aqueous solution is used to remove adsorbed pigments and impurities, a water-washing resin column is used to be neutral, aqueous methanol or ethanol is taken as an eluent, the eluent is distilled under reduced pressure, and residues are concentrated and evaporated to dryness to obtain the high-purity solid tea saponin. The resin used in the technical scheme of the invention needs to be firstly removed of adsorbed pigment and impurities by organic or inorganic alkaline aqueous solution and then washed to be neutral to elute the effective components, and the elution process is complex and the production period is long.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for extracting oil saponin from a camellia oleifera cake. The method comprises extracting with alkaline solution, adsorbing the obtained tea saponin crude product with special resin, eluting effective components with water after adsorption of resin column, and has the advantages of simple elution process, short production cycle, and high purity of the obtained product.
In order to solve the technical problems, the invention adopts the following technical scheme:
a method for extracting oil saponin from oil tea cakes comprises the following steps:
1) crushing the oil tea cake serving as a raw material, adding a solvent, heating and extracting for 1-2 times, filtering, and collecting an extracting solution; the solvent is sodium hydroxide aqueous solution, sodium carbonate aqueous solution, sodium bicarbonate aqueous solution or potassium carbonate aqueous solution with the pH value of 11-14;
2) adjusting the pH of the extracting solution to be less than or equal to 2 by using acid, stirring, standing, performing suction filtration, and collecting a filter cake;
3) dissolving the filter cake with water, passing through a macroporous resin column, washing the resin column with water until effluent liquid is colorless, eluting with ethanol or methanol with volume concentration of 60-80%, tracking and detecting by thin layer chromatography, and collecting alcohol eluent; the type of the macroporous resin
D-900, ADS-7 or LSA-700;
4) concentrating the eluate, adding a small amount of high-purity tea saponin into the concentrated solution, standing for crystallization, separating out crystals, and drying to obtain high-purity tea saponin.
In the technical proposal, the device comprises a base,
in the step 1), the oil tea cake is preferably crushed to 10 to 30 meshes. The adding amount of the solvent is 4-8 times of the weight of the raw materials in each extraction, the extraction time is 1-1.5 h, and the extraction temperature is usually 60-90 ℃.
In the step 2), the acid is sulfuric acid, hydrochloric acid, acetic acid or citric acid and other available acid solutions.
In the step 3), the flow rate is generally controlled to be 0.5-2 BV/h in the processes of sample introduction, column washing and elution.
In the step 4), the concentration is preferably performed until the concentration is 10 to 2 percent of the weight of the raw materials.
Compared with the prior art, the invention has the advantages that:
1. the alkali liquor is used as a solvent to extract the oil tea cake, so that the dissolution of the crude product of the tea saponin can be accelerated, and the production period is shortened;
2. the applicant finds that the resin model selected in the application has the decolorization effect while adsorbing the crude tea saponin, the selected resin can elute effective components after adsorbing the crude tea saponin by using a water washing column, and the obtained product has high purity and is white in color; in addition, the elution process is simple, so that the production period is shortened on the other hand;
3. the whole process is simple and easy to control, and the production cost is low.
Detailed Description
The present invention is further illustrated by the following specific examples, but the present invention is not limited to these examples.
1) Pulverizing oil tea cake to 20 mesh, taking 10kg, adding 8 times of sodium hydroxide solution (pH 11), heating to 80 deg.C, extracting for 1.5 hr, filtering, adding 4 times of sodium hydroxide solution (pH 11), heating to 80 deg.C, extracting for 1 hr, filtering, and mixing filtrates to obtain extractive solution;
2) regulating the pH value of the extracting solution to 1.5 by using sulfuric acid, stirring, standing, performing suction filtration, and collecting a filter cake;
3) heating the filter cake to 60 ℃ by using 20kg of purified water for dissolving, and passing through a D-900 macroporous resin column with the flow rate of 1.0 BV/h; washing the resin column with water until the effluent is colorless, eluting with 65% (v/v) ethanol at a flow rate of 2.0BV/h, detecting by thin layer chromatography, and collecting the ethanol eluate;
4) concentrating the eluate collected in step 3) under reduced pressure to 2.0kg, adding 20g high purity tea saponin (98.20%) into the obtained concentrated solution, standing for 12h for crystallization, vacuum filtering, and vacuum drying the obtained crystals at 60 deg.C under reduced pressure to obtain 1.10kg tea saponin.
The product was white crystals in appearance and 99% pure.
Claims (6)
1. The method for extracting oil saponin from the camellia oleifera cake is characterized by comprising the following steps of:
1) crushing the oil tea cake serving as a raw material, adding a solvent, heating and extracting for 1-2 times, filtering, and collecting an extracting solution; the solvent is sodium hydroxide aqueous solution, sodium carbonate aqueous solution, sodium bicarbonate aqueous solution or potassium carbonate aqueous solution with the pH value of 11-14;
2) adjusting the pH of the extracting solution to be less than or equal to 2 by using acid, stirring, standing, performing suction filtration, and collecting a filter cake;
3) dissolving the filter cake with water, passing through a macroporous resin column, washing the resin column with water until effluent liquid is colorless, eluting with ethanol or methanol with volume concentration of 60-80%, tracking and detecting by thin layer chromatography, and collecting alcohol eluent; the type of the macroporous resin
D-900, ADS-7 or LSA-700;
4) concentrating the eluate, adding a small amount of high-purity tea saponin into the concentrated solution, standing for crystallization, separating out crystals, and drying to obtain high-purity tea saponin.
2. The method for extracting oil saponin from the camellia oleifera cake as claimed in claim 1, wherein the method comprises the following steps: in the step 1), the oil tea cake is crushed to 10-30 meshes.
3. The method for extracting oil saponin from the camellia oleifera cake as claimed in claim 1, wherein the method comprises the following steps: the adding amount of the solvent is 4-8 times of the weight of the raw materials in each extraction, the extraction time is 1-1.5 h, and the extraction temperature is usually 60-90 ℃.
4. The method for extracting oil saponin from the camellia oleifera cake as claimed in claim 1, wherein the method comprises the following steps: in the step 2), the acid is sulfuric acid, hydrochloric acid, acetic acid or citric acid and other available acid solutions.
5. The method for extracting oil saponin from the camellia oleifera cake as claimed in claim 1, wherein the method comprises the following steps: in the step 3), the flow rate is generally controlled to be 0.5-2 BV/h in the processes of sample introduction, column washing and elution.
6. The method for extracting oil saponin from the camellia oleifera cake as claimed in claim 1, wherein the method comprises the following steps: in the step 4), the concentration is preferably performed until the concentration is 10 to 2 percent of the weight of the raw materials.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911386994.4A CN111018940A (en) | 2019-12-29 | 2019-12-29 | Method for extracting oil saponin from oil-tea camellia cakes |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911386994.4A CN111018940A (en) | 2019-12-29 | 2019-12-29 | Method for extracting oil saponin from oil-tea camellia cakes |
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| Publication Number | Publication Date |
|---|---|
| CN111018940A true CN111018940A (en) | 2020-04-17 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911386994.4A Withdrawn CN111018940A (en) | 2019-12-29 | 2019-12-29 | Method for extracting oil saponin from oil-tea camellia cakes |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112047995A (en) * | 2020-09-24 | 2020-12-08 | 深圳市天同玩具有限公司 | Tea saponin draws equipment |
| CN113087813A (en) * | 2021-03-17 | 2021-07-09 | 广州芊亮科技有限公司 | Tea bran extraction process |
-
2019
- 2019-12-29 CN CN201911386994.4A patent/CN111018940A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112047995A (en) * | 2020-09-24 | 2020-12-08 | 深圳市天同玩具有限公司 | Tea saponin draws equipment |
| CN113087813A (en) * | 2021-03-17 | 2021-07-09 | 广州芊亮科技有限公司 | Tea bran extraction process |
| CN113087813B (en) * | 2021-03-17 | 2021-11-02 | 广州芊亮科技有限公司 | Tea bran extraction process |
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Application publication date: 20200417 |