CN106967144A - A kind of method that Tea Saponin is extracted from tea bran - Google Patents
A kind of method that Tea Saponin is extracted from tea bran Download PDFInfo
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- CN106967144A CN106967144A CN201710192863.7A CN201710192863A CN106967144A CN 106967144 A CN106967144 A CN 106967144A CN 201710192863 A CN201710192863 A CN 201710192863A CN 106967144 A CN106967144 A CN 106967144A
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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 belongs to Tea Saponin preparing technical field, more particularly to a kind of method that Tea Saponin is extracted from tea bran comprises the following steps:Crushing, HIGH PRESSURE TREATMENT, ultrasonically treated, alcohol precipitation, concentration, drying, be specially:1) dry tea bran is taken to carry out pulverization process;2) the tea bran after crushing is subjected to HIGH PRESSURE TREATMENT;3) the tea bran after HIGH PRESSURE TREATMENT is subjected to ultrasonic wave extraction;4) alcohol precipitation, is concentrated, and is dried.The inventive method uses the combination of HIGH PRESSURE TREATMENT, ultrasonic wave extraction and alcohol precipitation technology, not only improves the recovery rate and purity of Tea Saponin, but also substantially reduces manufacturing cycle, improves productivity ratio.
Description
Technical field
The invention belongs to Tea Saponin preparing technical field, more particularly to a kind of method that Tea Saponin is extracted from tea bran.
Background technology
Tea bran, alias tea seed cake, tea seed cake, major product of the tea seed after processing is tea oil, extracts the pair after tea oil
Product is referred to as tea bran, and it is mainly made up of fiber, protein, Tea Saponin, starch sugar and the thing that spreads out altogether.The day of high-quality is rich in tea bran
Right Tea Saponin, content is about 12~20% or so.Tea Saponin (teasaponin) is alkaloid, and 223~224 DEG C of fusing point is easily inhaled
Wet, bitter is peppery, can be dissolved in the intensive polar solvents such as water, methanol, ethanol, acetic acid, pyridine, has insoluble in ether, petroleum ether, benzene etc.
Machine solvent.The terpenoid of three ring five that Tea Saponin is made up of aglucon, sugared body and organic acid, with stronger adhesive force, emulsification
Power, dispersion force, wetting power and foaming power.Tea Saponin has high toxicity to cold-blooded animal, and then nontoxic to homeothermal animals such as people and animals
Or low toxicity.Therefore Tea Saponin can be replaced and part replaces application of the chemical products in veterinary drug and agricultural chemicals, with the anti-of its uniqueness
The mechanism of action of microorganism, parasite and insect, will not cause organism to develop immunity to drugs and drug resistance, and people and animals will not be produced
Harmful effect, can be used for a long time.In addition, the Tea Saponin in tea bran, is a kind of excellent nonionic nature surface activating agent, has
The effects such as hair washing, hair care, black hair and anti-dandruff, Anti-hair loss.
The extractive technique method of current natural tea saponin powder, the raw material of extraction is had nothing in common with each other, and is mainly manifested in extraction production work
In terms of skill is different, to extract preparing raw material different, the deficiency existed is mainly manifested in that recovery rate is relatively low, product purity is not high,
Production cost is excessive etc., is very different with the present invention.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of method that Tea Saponin is extracted from tea bran, the tea prepared
Saponin recovery rate and purity are high.
To achieve the above object, technical scheme to be solved by this invention is:
The present invention provides a kind of method that Tea Saponin is extracted from tea bran, comprises the following steps:Crushing, HIGH PRESSURE TREATMENT, ultrasound
Processing, alcohol precipitation, concentration, drying, be specially:
1) dry tea bran is taken to carry out pulverization process;
2) the tea bran after crushing is subjected to HIGH PRESSURE TREATMENT;
3) the tea bran after HIGH PRESSURE TREATMENT is subjected to ultrasonic wave extraction;
4) alcohol precipitation, is concentrated, and is dried.
Step 1 of the present invention) in, tea bran is crushed to 100~200 mesh.
Step 2 of the present invention) in, add ethanol solution, 3~8min of HIGH PRESSURE TREATMENT under 35~43MPa pressure.So
Under conditions of, the recovery rate and purity of Tea Saponin can be improved.
The volume ratio of ethanol solution of the present invention and tea bran is 3~5:1.In the range of this solid-liquid ratio, Tea Saponin
Recovery rate have obvious increase, when solid-liquid ratio superelevation 1:When 5, the recovery rate of Tea Saponin is not significantly increased, and is considered
Solvent cost in recovery rate and extraction process, solid-liquid ratio is 1:5 be most suitable.
The volumetric concentration of ethanol solution of the present invention is 55%~70%.In this volume concentration range, Tea Saponin
Recovery rate slow rise, but after volumetric concentration is higher than 70%, the recovery rate of Tea Saponin declines.
Temperature during HIGH PRESSURE TREATMENT of the present invention is 45~55 DEG C.Extract in this temperature range, Tea Saponin is carried
Take rate higher, more than this temperature range, Tea Saponin is difficult to extract, recovery rate reduction.
Step 3 of the present invention) in, 30~50min of ultrasonication under 220~280 power.This extraction conditions temperature
With, by HIGH PRESSURE TREATMENT above, then carry out ultrasonic wave extraction, be conducive to improve Tea Saponin recovery rate and purity.
Temperature during ultrasonication of the present invention is 35~45 DEG C.Extracted in this temperature range, the extraction of Tea Saponin
Rate and purity are higher, more than this temperature range, recovery rate reduction.
Step 4 of the present invention) in, alcohol precipitation is specially:The solution obtained after ultrasonic wave extraction is taken, its weight 2~3 is added
Times methanol solution, stirs, and standing makes layering, filters.Tea Saponin can be further purified in alcohol precipitation, remove impurity, improve tea
The purity of saponin.
The volumetric concentration of methanol solution of the present invention is 80%~90%.In this volume concentration range, more favorably
In the purifying of Tea Saponin, impurity is removed.
Using the inventive method from tea bran extract Tea Saponin, compared with prior art, have the advantage that for:
1st, prior art is when carrying out Tea Saponin extraction, and pre-treatment is typically all for solvent, by adding with water or ethanol etc.
Heat is extracted active ingredient dissolution, and the present invention passes through HIGH PRESSURE TREATMENT so that tissue cellularity is suitably squeezed in tea bran
Compressive strain, promotes the diffusion between solute and solution, Tea Saponin active ingredient is better contacted with Extraction solvent, molten
Solution, improves recovery rate, is conducive to ultrasonic wave and the alcohol precipitation processing of subsequent technique, beneficial to raising Tea Saponin purity.
2nd, prior art extracts Tea Saponin recovery rate and is generally 95.2%, and is difficult to ensure Tea Saponin under high extraction
High-purity, and the present invention is using the combination of HIGH PRESSURE TREATMENT, ultrasonic wave extraction and alcohol precipitation technology so that technology of the invention combines
The raising of existing matter, the present invention extracts Tea Saponin extraction rate reached to more than 97%, and purity is high, reaches more than 93.2%.
3rd, the combination of HIGH PRESSURE TREATMENT of the invention, ultrasonic wave extraction and alcohol precipitation technology, not only improves the recovery rate of Tea Saponin
And purity, but also manufacturing cycle is substantially reduced, improve productivity ratio.
Embodiment
The invention will be further described with reference to embodiments, but the invention is not limited in these embodiments.
Embodiment 1
A kind of method that Tea Saponin is extracted from tea bran, comprises the following steps:
1) dry tea bran is taken to be crushed to 180 mesh;
2) by the tea bran after crushing, the volumetric concentration for adding 3 times of tea bran volume is 65% ethanol solution, in 35MPa pressures
HIGH PRESSURE TREATMENT 3min at a temperature of power and 45 DEG C;
3) by the tea bran after HIGH PRESSURE TREATMENT, the ultrasonic wave extraction 30min at a temperature of 220 power and 35 DEG C;
4) solution obtained after ultrasonic wave extraction is taken, 2 times of its weight is added, volumetric concentration is 80% methanol solution, stirring
Uniformly, standing makes layering, filters, and it is 1.2 to be concentrated into relative density, spray drying.
After testing, the recovery rate for preparing Tea Saponin is 97.1%, and purity is 93.5%.
Embodiment 2
A kind of method that Tea Saponin is extracted from tea bran, comprises the following steps:
1) dry tea bran is taken to be crushed to 100 mesh;
2) by the tea bran after crushing, the volumetric concentration for adding 4 times of tea bran volume is 65% ethanol solution, in 37MPa pressures
HIGH PRESSURE TREATMENT 5min at a temperature of power and 48 DEG C;
3) by the tea bran after HIGH PRESSURE TREATMENT, the ultrasonic wave extraction 35min at a temperature of 230 power and 38 DEG C;
4) solution obtained after ultrasonic wave extraction is taken, 3 times of its weight is added, volumetric concentration is 85% methanol solution, stirring
Uniformly, standing makes layering, filters, and it is 1.2 to be concentrated into relative density, spray drying.
After testing, the recovery rate for preparing Tea Saponin is 97%, and purity is 93.5%.
Embodiment 3
A kind of method that Tea Saponin is extracted from tea bran, comprises the following steps:
1) dry tea bran is taken to be crushed to 120 mesh;
2) by the tea bran after crushing, the volumetric concentration for adding 5 times of tea bran volume is 70% ethanol solution, in 40MPa pressures
HIGH PRESSURE TREATMENT 6min at a temperature of power and 50 DEG C;
3) by the tea bran after HIGH PRESSURE TREATMENT, the ultrasonic wave extraction 40min at a temperature of 240 power and 40 DEG C;
4) solution obtained after ultrasonic wave extraction is taken, 2 times of its weight is added, volumetric concentration is 85% methanol solution, stirring
Uniformly, standing makes layering, filters, and it is 1.2 to be concentrated into relative density, spray drying.
After testing, the recovery rate for preparing Tea Saponin is 97.3%, and purity is 93.2%.
Embodiment 4
A kind of method that Tea Saponin is extracted from tea bran, comprises the following steps:
1) dry tea bran is taken to be crushed to 150 mesh;
2) by the tea bran after crushing, the volumetric concentration for adding 3 times of tea bran volume is 60% ethanol solution, in 43MPa pressures
HIGH PRESSURE TREATMENT 7min at a temperature of power and 52 DEG C;
3) by the tea bran after HIGH PRESSURE TREATMENT, the ultrasonic wave extraction 45min at a temperature of 260 power and 43 DEG C;
4) solution obtained after ultrasonic wave extraction is taken, 3 times of its weight is added, volumetric concentration is 90% methanol solution, stirring
Uniformly, standing makes layering, filters, and it is 1.2 to be concentrated into relative density, spray drying.
After testing, the recovery rate for preparing Tea Saponin is 97.2%, and purity is 93.4%.
Embodiment 5
A kind of method that Tea Saponin is extracted from tea bran, comprises the following steps:
1) dry tea bran is taken to be crushed to 200 mesh;
2) by the tea bran after crushing, the volumetric concentration for adding 4 times of tea bran volume is 55% ethanol solution, in 43MPa pressures
HIGH PRESSURE TREATMENT 8min at a temperature of power and 55 DEG C;
3) by the tea bran after HIGH PRESSURE TREATMENT, the ultrasonic wave extraction 50min at a temperature of 280 power and 45 DEG C;
4) solution obtained after ultrasonic wave extraction is taken, 2 times of its weight is added, volumetric concentration is 90% methanol solution, stirring
Uniformly, standing makes layering, filters, and it is 1.2 to be concentrated into relative density, spray drying.
After testing, the recovery rate for preparing Tea Saponin is 97.4%, and purity is 93.2%.
Prior art:Adopt new technology extraction Tea Saponin, i.e. water extraction and alcohol precipitation method.The optimum process condition of water extraction process is leaching
Carry temperature 60 C, liquid-solid ratio 10:1, extraction time 2h, extracting times 3 times.Alcohol precipitation again after water is extracted, is obtained most by experiment
Excellent condition is concentration of alcohol 90%, ethanol and concentrate volume ratio 4:1st, 75 DEG C of alcohol precipitation temperature, alcohol precipitation time 2.5h, and at this
Compare water extraction and water extraction and alcohol precipitation method under part, it is 95.2% to draw water extraction and alcohol precipitation method recovery rate, and purity is 69.9%, is improved pure
Degree, is conducive to follow-up refinement treatment.
Claims (10)
1. a kind of method that Tea Saponin is extracted from tea bran, it is characterised in that comprise the following steps:Crushing, HIGH PRESSURE TREATMENT, ultrasound at
Reason, alcohol precipitation, concentration, drying, be specially:
1) dry tea bran is taken to carry out pulverization process;
2) the tea bran after crushing is subjected to HIGH PRESSURE TREATMENT;
3) the tea bran after HIGH PRESSURE TREATMENT is subjected to ultrasonic wave extraction;
4) alcohol precipitation, is concentrated, and is dried.
2. the method according to claim 1 that Tea Saponin is extracted from tea bran, it is characterised in that:The step 1) in, tea bran
It is crushed to 100~200 mesh.
3. the method according to claim 1 that Tea Saponin is extracted from tea bran, it is characterised in that:The step 2) in, add
Ethanol solution, 3~8min of HIGH PRESSURE TREATMENT under 35~43MPa pressure.
4. the method according to claim 3 that Tea Saponin is extracted from tea bran, it is characterised in that:The ethanol solution and tea bran
Volume ratio be 3~5:1.
5. the method according to claim 4 that Tea Saponin is extracted from tea bran, it is characterised in that:The volume of the ethanol solution
Concentration is 55%~70%.
6. the method that Tea Saponin is extracted from tea bran according to Claims 1 to 5 any one, it is characterised in that:The height
Temperature during pressure processing is 45~55 DEG C.
7. the method according to claim 1 that Tea Saponin is extracted from tea bran, it is characterised in that:The step 3) in, 220
30~50min of ultrasonic wave extraction under~280 power.
8. the method according to claim 7 that Tea Saponin is extracted from tea bran, it is characterised in that:Temperature during ultrasonication
For 35~45 DEG C.
9. the method according to claim 1 that Tea Saponin is extracted from tea bran, it is characterised in that:The step 4) in, alcohol precipitation
Specially:The solution obtained after ultrasonic wave extraction is taken, 2~3 times of methanol solutions of its weight is added, stirs, standing makes layering,
Filtering.
10. the method according to claim 9 that Tea Saponin is extracted from tea bran, it is characterised in that:The body of the methanol solution
Product concentration is 80%~90%.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108640966A (en) * | 2018-07-23 | 2018-10-12 | 广西壮族自治区农业科学院农产品加工研究所 | A kind of eutectic solvent and extraction process for extracting Tea Saponin in leached tea oil slag |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108640966A (en) * | 2018-07-23 | 2018-10-12 | 广西壮族自治区农业科学院农产品加工研究所 | A kind of eutectic solvent and extraction process for extracting Tea Saponin in leached tea oil slag |
CN108640966B (en) * | 2018-07-23 | 2021-02-02 | 广西壮族自治区农业科学院农产品加工研究所 | Eutectic solvent for extracting tea saponin from tea seed meal and extraction process |
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