CN102603857A - Method for extracting tea saponin from camellia oleifera cake - Google Patents
Method for extracting tea saponin from camellia oleifera cake Download PDFInfo
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- CN102603857A CN102603857A CN2012100502009A CN201210050200A CN102603857A CN 102603857 A CN102603857 A CN 102603857A CN 2012100502009 A CN2012100502009 A CN 2012100502009A CN 201210050200 A CN201210050200 A CN 201210050200A CN 102603857 A CN102603857 A CN 102603857A
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Abstract
The invention discloses a method for extracting tea saponin from a camellia oleifera cake. The method comprises the following steps of: (1) smashing the camellia oleifera cake, adding a solvent, heating and extracting for once to twice, and collecting an extracting solution, wherein the solvent is a sodium hydrate aqueous solution, a sodium carbonate aqueous solution, a sodium bicarbonate aqueous solution or a potassium carbonate aqueous solution of which the pH is equal to 11-14; (2) adjusting the pH of the extracting solution to be less than or equal to 2, 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 till an effluent is colorless, eluting with ethanol or methanol of which the volume concentration is 60-80 percent, tracking and detecting through thin-layer chromatography, and collecting an alcohol eluent, wherein the model of macroporous resin is D-900, ADS-7 or LSA-700; and (4) concentrating the eluent, adding a small amount of high-purity tea saponin into a concentrated solution, standing for devitrifying, separating a crystal out, and drying to obtain the tea saponin. The method disclosed by the invention has the advantages of simple and easily-controllable process, short production period, low production cost and high product purity.
Description
Technical field
The present invention relates to the preparation method of tea saponin, be specifically related to from the oil tea cake, extract the method for tea saponin.
Background technology
The oil tea cake is Theaceae, and oil tea belongs to the pie residue that is pressed into after the kind benevolence oil expression of evergreen dungarunga tea oil tree (Camellia oleiferaAbel).The oil tea cake contains fat, protein, robust fibre, tea saponin, carbohydrate and a spot of Polyphenols anti-oxidation active substance, can therefrom extract materials such as Residual oil, tea saponin, polyphenol, and the content of tea saponin is up to 15% in the oil tea cake.Tea saponin has another name called the tea saponin, belongs to the triterpenes saponin, has the toil pungent, stimulates nasal membrane to cause sneeze, and pure article are white fine columnar crystal, and water absorbability is strong; Be a kind of well behaved natural type of candy glucoside compound tensio-active agent, it can be widely used in fields such as light industry, chemical industry, agricultural chemicals, feed, breed, weaving, oil recovery, mining, building materials and expressway construction, and economic worth is than higher.
Publication number is the patent of invention of CN1148598, discloses a kind of method of extracting refined theasapogenin, is to be raw material with the oil tea cake; Adopt the tea saponin in the homemade styrene type copolymer resins absorption tea cake leaching liquid; Removing pigment and the impurity that is adsorbed with the organic or inorganic alkali aqueous solution, is elutriant with aqueous methanol or ethanol again after washed resin post to the neutrality, the underpressure distillation elutriant; Residue concentrates evaporate to dryness, promptly gets highly purified solid tea saponin.This invents the resin that uses in the said technical scheme, needs to remove pigment and the impurity that is adsorbed with the organic or inorganic alkali aqueous solution earlier, washes to neutrality again and just effective constituent is carried out wash-out, and elution process is loaded down with trivial details, and the production cycle is longer.
Summary of the invention
The technical problem that the present invention will solve provides a kind of method of from the oil tea cake, extracting tea saponin.This method is extracted with alkali lye earlier; Gained tea saponin bullion selects for use the resin of special type that the tea saponin bullion is adsorbed, and resin column only needs water flushing back just can carry out wash-out to effective constituent after absorption, and elution process is simple; With short production cycle, products obtained therefrom purity is high.
For solving the problems of the technologies described above, the present invention adopts following technical scheme:
From the oil tea cake, extract the method for tea saponin, may further comprise the steps:
1) is raw material with the oil tea cake, pulverizes, add the solvent heating and extracting 1～2 time, filter, collect extracting solution; Described solvent is aqueous sodium hydroxide solution, aqueous sodium carbonate, sodium bicarbonate aqueous solution or the wet chemical of pH=11～14;
2) with pH≤2 of acid adjusting extracting solution, stir, leave standstill, suction filtration is collected filter cake;
3) filter cake is crossed macroporous resin column after with water dissolution, and is colourless with washing resin column to effluent earlier, and using volumetric concentration again is 60～80% ethanol or methanol-eluted fractions, and thin-layer chromatography is followed the tracks of and detected, and collects alcohol eluen; The model of said macroporous resin is D-900, ADS-7 or LSA-700;
4) elutriant concentrates, and adds a small amount of high-purity tea saponin in the liquid concentrator, places crystallization, isolates crystal, and drying obtains highly purified tea saponin.
In the technique scheme,
In the step 1), preferably the oil tea cake is crushed to 10～30 orders.The add-on of solvent is 4～8 times of raw material weight during each the extraction, and the time of extraction is 1～1.5h, and the temperature of extraction is generally 60～90 ℃.
Step 2) in, described acid is other available acid solutions such as sulfuric acid, hydrochloric acid, acetic acid or Hydrocerol A.
In the step 3), at sample introduction, wash in the process of post and wash-out, flow velocity generally is controlled at 0.5～2BV/h.
In the step 4), described concentrating preferably is concentrated into 10～20% of raw material weight.
Compared with prior art, the invention has the advantages that:
1, is that solvent extracts the stripping that can accelerate the tea saponin bullion to the oil tea cake with alkali lye, thereby shortens the production cycle;
2, the applicant finds through test of long duration; The resin model of being selected for use among the application is in the effect that the absorption of tea saponin bullion is had simultaneously concurrently decolouring; The resin of being selected for use adsorbs the back to the tea saponin bullion only to be needed with just carrying out wash-out to effective constituent behind the washing post; And products obtained therefrom purity is high, and color is a white; In addition, because elution process is simple, shorten the production cycle from another point of view;
3, whole technology is simple and easy to control, and production cost is low.
Embodiment
With specific embodiment the present invention is described further below, but the present invention is not limited to these embodiment.
Embodiment 1
1) the oil tea cake is crushed to 20 orders, gets 10kg, the sodium hydroxide solution (pH=11) that adds 8 times of raw material weights is heated to 80 ℃ and extracts 1.5h; Filter, the sodium hydroxide solution (pH=11) that filter residue adds 4 times of raw material weights again is heated to 80 ℃ of extraction 1h, filters; Merging filtrate gets extracting solution;
2) with the pH value to 1.5 of sulfuric acid adjusting extracting solution, stir, leave standstill, suction filtration is collected filter cake;
3) filter cake is heated to 60 ℃ of dissolvings with the 20kg pure water, crosses the D-900 macroporous resin column, advances column flow rate 1.0BV/h; Washed resin post to effluent is colourless, and flow velocity 2.0BV/h uses 65% (v/v) ethanol elution then, and flow velocity 1.0BV/h, thin-layer chromatography follow the tracks of and detect, and collect alcohol eluen;
4) elutriant of step 3) being collected is evaporated to 2.0kg, adds 20g high-purity tea saponin (98.20%) in the gained liquid concentrator, places the 12h crystallization, suction filtration, and the gained crystal is dry at 60 ℃ of following vacuum decompressions, gets tea saponin 1.10kg.
The products obtained therefrom outward appearance is a white crystal, and purity is 99.10%.
Embodiment 2
1) the oil tea cake is crushed to 30 orders, gets 50kg, the sodium carbonate solution (pH=13) that adds 6 times of raw material weights is heated to 70 ℃ and extracts 1h; Filter, the sodium hydroxide solution (pH=13) that filter residue adds 4 times of raw material weights again is heated to 70 ℃ of extraction 1h, filters; Merging filtrate gets extracting solution;
2) with the pH value to 2 of hydrochloric acid adjusting extracting solution, stir, leave standstill, suction filtration is collected filter cake;
3) filter cake is heated to 60 ℃ of dissolvings with the 80kg pure water, crosses the ADS-7 macroporous resin column, advances column flow rate 1.0BV/h; Washed resin post to effluent is colourless, and flow velocity 1.0BV/h uses 75% (v/v) methanol-eluted fractions then, and flow velocity 1.0BV/h, thin-layer chromatography follow the tracks of and detect, and collect alcohol eluen;
4) elutriant of step 3) being collected is evaporated to 9.0kg, adds 150g high-purity tea saponin (98.20%) in the gained liquid concentrator, places the 24h crystallization, suction filtration, and the gained crystal is dry at 65 ℃ of following vacuum decompressions, gets tea saponin 5.0kg.
The products obtained therefrom outward appearance is a white crystal, and purity is 99.25%.
Embodiment 3
1) the oil tea cake is crushed to 20 orders, gets 80kg, the sodium hydrogen carbonate solution (pH=14) that adds 5 times of raw material weights is heated to 60 ℃ and extracts 1h; Filter, the sodium hydroxide solution (pH=14) that filter residue adds 6 times of raw material weights again is heated to 75 ℃ of extraction 1h, filters; Merging filtrate gets extracting solution;
2) with the pH value to 1.0 of sulfuric acid adjusting extracting solution, stir, leave standstill, suction filtration is collected filter cake;
3) filter cake is heated to 60 ℃ of dissolvings with the 90kg pure water, crosses the LSA-700 macroporous resin column, advances column flow rate 1.5BV/h; Washed resin post to effluent is colourless, and flow velocity 2.0BV/h uses 80% (v/v) methanol-eluted fractions then, and flow velocity 1.0BV/h, thin-layer chromatography follow the tracks of and detect, and collect alcohol eluen;
4) elutriant of step 3) being collected is evaporated to 12.0kg, adds 120g high-purity tea saponin (98.20%) in the gained liquid concentrator, places the 18h crystallization, suction filtration, and the gained crystal is dry at 60 ℃ of following vacuum decompressions, gets tea saponin 9.5kg.
The products obtained therefrom outward appearance is a white crystal, and purity is 98.55%.
Embodiment 4
1) the oil tea cake is crushed to 10 orders, gets 100kg, the solution of potassium carbonate (pH=11) that adds 8 times of raw material weights is heated to 80 ℃ and extracts 1.5h, filters, and filtrating is extracting solution;
2) with the pH value to 0.8 of acetic acid adjusting extracting solution, stir, leave standstill, suction filtration is collected filter cake;
3) filter cake is heated to 65 ℃ of dissolvings with the 120kg pure water, crosses the D-900 macroporous resin column, advances column flow rate 1.0BV/h; Washed resin post to effluent is colourless, and flow velocity 2.0BV/h uses 70% (v/v) ethanol elution then, and flow velocity 0.8BV/h, thin-layer chromatography follow the tracks of and detect, and collect alcohol eluen;
4) elutriant of step 3) being collected is evaporated to 15.0kg, adds 100g high-purity tea saponin (98.20%) in the gained liquid concentrator, places the 30h crystallization, suction filtration, and the gained crystal is dry at 65 ℃ of following vacuum decompressions, gets tea saponin 12.6kg.
The products obtained therefrom outward appearance is a white crystal, and purity is 99.31%.
Embodiment 5
1) the oil tea cake is crushed to 30 orders, gets 200kg, the sodium hydroxide solution (pH=12) that adds 6 times of raw material weights is heated to 75 ℃ and extracts 1.5h, filters, and filtrating is extracting solution;
2) with the pH value to 1.8 of Hydrocerol A adjusting extracting solution, stir, leave standstill, suction filtration is collected filter cake;
3) filter cake is heated to 60 ℃ of dissolvings with the 18kg pure water, crosses the ADS-7 macroporous resin column, advances column flow rate 2.0BV/h; Washed resin post to effluent is colourless, and flow velocity 2.0BV/h uses 60% (v/v) ethanol elution then, and flow velocity 1.0BV/h, thin-layer chromatography follow the tracks of and detect, and collect alcohol eluen;
4) elutriant of step 3) being collected is evaporated to 3.5kg, adds 20g high-purity tea saponin (98.20%) in the gained liquid concentrator, places the 48h crystallization, suction filtration, and the gained crystal is dry at 70 ℃ of following vacuum decompressions, gets tea saponin 1.9kg.
The products obtained therefrom outward appearance is a white crystal, and purity is 99.05%.
Claims (5)
1. from the oil tea cake, extract the method for tea saponin, it is characterized in that may further comprise the steps:
1) is raw material with the oil tea cake, pulverizes, add the solvent heating and extracting 1～2 time, filter, collect extracting solution; Described solvent is aqueous sodium hydroxide solution, aqueous sodium carbonate, sodium bicarbonate aqueous solution or the wet chemical of pH=11～14;
2) with pH≤2 of acid adjusting extracting solution, stir, leave standstill, suction filtration is collected filter cake;
3) filter cake is crossed macroporous resin column after with water dissolution, and is colourless with washing resin column to effluent earlier, and using volumetric concentration again is 60～80% ethanol or methanol-eluted fractions, and thin-layer chromatography is followed the tracks of and detected, and collects alcohol eluen; The model of said macroporous resin is D-900, ADS-7 or LSA-700;
4) elutriant concentrates, and adds a small amount of high-purity tea saponin in the liquid concentrator, places crystallization, isolates crystal, and drying obtains highly purified tea saponin.
2. the method for from the oil tea cake, extracting tea saponin according to claim 1 is characterized in that: in the step 1), the add-on of solvent is 4～8 times of raw material weight when extracting at every turn, and the time of extraction is 1～1.5h.
3. the method for from the oil tea cake, extracting tea saponin according to claim 1 is characterized in that: in the step 1), and said raw material pulverizing to 10～30 orders.
4. the method for from the oil tea cake, extracting tea saponin according to claim 1 is characterized in that: step 2) in, described acid is sulfuric acid, hydrochloric acid, acetic acid or Hydrocerol A.
5. the method for from the oil tea cake, extracting tea saponin according to claim 1, it is characterized in that: in the step 4), described simmer down to is concentrated into 10～20% of raw material weight.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2012100502009A CN102603857A (en) | 2012-02-29 | 2012-02-29 | Method for extracting tea saponin from camellia oleifera cake |
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| CN2012100502009A CN102603857A (en) | 2012-02-29 | 2012-02-29 | Method for extracting tea saponin from camellia oleifera cake |
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| CN102603857A true CN102603857A (en) | 2012-07-25 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102993329A (en) * | 2012-12-31 | 2013-03-27 | 广西师范大学 | Method for comprehensively extracting saponin, polysaccharides and polyphenol from camellia oleifera abel defatted cakes |
| CN104530173A (en) * | 2014-12-11 | 2015-04-22 | 福建华仁油脂有限公司 | Process for extracting tea saponin from oil tea cake |
| CN104961793A (en) * | 2015-06-29 | 2015-10-07 | 兰捷 | Method for extracting high-purity tea saponin from tea seed cake dregs |
| CN113264976A (en) * | 2021-05-31 | 2021-08-17 | 湖南万象生物科技有限公司 | High-purity tea saponin sodium and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1148598A (en) * | 1995-10-25 | 1997-04-30 | 西南石油学院 | Method for extracting refined theasapogenin |
-
2012
- 2012-02-29 CN CN2012100502009A patent/CN102603857A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1148598A (en) * | 1995-10-25 | 1997-04-30 | 西南石油学院 | Method for extracting refined theasapogenin |
Non-Patent Citations (2)
| Title |
|---|
| 殷肇君等: "油茶粕中茶皂素的提取及纯化研究", 《饲料工业》 * |
| 赵晓东: "一种纯化茶皂素的方法", 《西南石油学院学报》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102993329A (en) * | 2012-12-31 | 2013-03-27 | 广西师范大学 | Method for comprehensively extracting saponin, polysaccharides and polyphenol from camellia oleifera abel defatted cakes |
| CN104530173A (en) * | 2014-12-11 | 2015-04-22 | 福建华仁油脂有限公司 | Process for extracting tea saponin from oil tea cake |
| CN104961793A (en) * | 2015-06-29 | 2015-10-07 | 兰捷 | Method for extracting high-purity tea saponin from tea seed cake dregs |
| CN113264976A (en) * | 2021-05-31 | 2021-08-17 | 湖南万象生物科技有限公司 | High-purity tea saponin sodium and preparation method thereof |
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Application publication date: 20120725 |