CN113024629A - Tea saponin purification method - Google Patents
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- C07H1/00—Processes for the preparation of sugar derivatives
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- C07H1/08—Separation; Purification from natural products
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Abstract
The invention relates to the technical field of tea saponin, in particular to a tea saponin purification method. The method comprises the following steps: (1) processing oil tea seed meal, (2) extracting tea saponin roughly, and (3) refining the tea saponin roughly. According to the invention, the camellia seed meal is dried after being crushed, and impurities in the camellia seed meal are further removed, so that the material has large gaps and more space for contacting a solvent; the camellia seed meal is decomposed by mixing water and adding enzyme, so that the cell molecular structure of the camellia seed meal is dispersed, and the infiltration effect of a solvent is improved; then spray drying to evaporate water and keep the components of the material intact. The extraction solvent formed by mixing the deionized water, the absolute ethyl alcohol and the ethyl acetate is used, so that the soluble target range is expanded, the tea saponin combined with other water-soluble and alcohol-soluble substances can be extracted more conveniently, the extraction rate of the tea saponin can be obviously improved, and the prepared tea saponin has higher activity and more purposes.
Description
Technical Field
The invention relates to the technical field of tea saponin, in particular to a tea saponin purification method.
Background
The oil tea is a basic edible oil tree species in China, and simultaneously, China is also the country with the largest area for cultivating the oil tea in the world. The camellia seed meal contains 10-16% of tea saponin, is an important source of the tea saponin, contains abundant polysaccharide and protein and is an excellent feed.
With the development of industrial extraction and application research of tea saponin, the production process of tea saponin is continuously improved, but has not made a great breakthrough so far. The conventional extraction process mainly comprises water extraction, hydrous ethanol, hydrous methanol and other extraction processes, and particularly adopts auxiliary measures such as supercritical extraction, microbial decomposition and the like. For example, a preparation method of natural high-purity tea saponin with high-efficiency decontamination, which is disclosed in the patent No. CN201711296589.4, comprises the steps of firstly extracting tea saponin from tea seed meal by adopting a microwave-ultrasonic wave auxiliary combined double-aqueous phase extraction technology; then removing strong polar impurities in the tea saponin by adopting a low co-melting reagent-salt aqueous two-phase extraction technology, thereby improving the purity of the tea saponin; and finally, further purifying the tea saponin by using a supercritical CO2 extraction technology to obtain the high-purity natural tea saponin. The method is environment-friendly and simple to operate, equipment is complex, the method is not suitable for most people to use, the solubility of the supercritical extraction is extremely high, the accuracy in a small range is poor when the supercritical extraction is carried out, and a plurality of structural analogs are easily wrapped; for another example, CN201911294499.0 discloses a method for rapidly refining tea saponin, which comprises the steps of firstly, rapidly extracting tea saponin with aqueous ethanol at a lower temperature, concentrating and removing organic solvent, then, separating most polar impurities by using a small-molecular organic solvent-salt aqueous two-phase extraction system, finally removing salt and organic solvent, and drying to obtain a high-purity tea saponin product.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a tea saponin purification method to improve the yield and purity of tea saponin, which comprises the following steps:
(1) oil tea seed meal treatment
Crushing the camellia seed meal into powder of 100-plus 200 meshes, drying for 3-5h at 15-20 ℃ under 0.1-0.3 standard atmospheric pressure, mixing the powder with purified water of which the mass is 10-13 times of that of the powder, adjusting the ph of the mixed solution to 5.3-5.5 by using an acetic acid solution, adding cellulase of which the mass is 5-8% of that of the mixed solution, stirring for 50-80min at 40-45 ℃ at 80-200r/min, adjusting the ph of the mixed solution to 8-8.5 by using a calcium hydroxide solution, adding protease of which the mass is 2-3% of that of the mixed solution, stirring for 30-50min at 53-55 ℃ at 100-150r/min, spray-drying the mixed solution, and drying for 30-50min at 15-20 ℃ under 0.01-0.03 standard atmospheric pressure to obtain the enzymolysis camellia seed meal;
(2) crude extraction of tea saponin
Mixing the enzymatic hydrolysis camellia seed meal with an extraction solvent, stirring for 5-8min at 20-25 ℃ at 500r/min, standing for 1-3h, introducing carbon dioxide, sealing, soaking at 30-35 ℃ for 30-50min, heating to 43-45 ℃ by microwave, preserving heat for 10-15min, naturally cooling the mixed system to room temperature, heating to 38-43 ℃ by microwave, preserving heat for 20-30min, and filtering; drying the filtrate under reduced pressure, mixing the obtained powder with n-butanol 10-20 times the weight of the powder at 40-45 deg.C, soaking for 20-30min, filtering, and drying the filtrate under reduced pressure to obtain crude product of tea saponin;
(3) refining tea saponin crude product
Mixing the crude product of tea saponin with benzene 8-10 times of the mass of the crude product, stirring at high speed of 900r/min at 40-50 ℃ for 10-15min, standing for 3-5h, filtering, and drying the filter residue under reduced pressure; mixing the obtained dry product with 10-20 times of acetic acid, standing for 30-50min, filtering, and drying under reduced pressure to obtain purified tea saponin.
Further, in the step (1), the mass fraction of the acetic acid solution is 8-12%.
Further, in the step (1), the mass fraction of the calcium hydroxide solution is 0.3-0.5%.
Further, in the step (2), the extraction solvent is formed by mixing deionized water, absolute ethyl alcohol and ethyl acetate according to the mass ratio of 3-5:5-8: 1-2.
Further, in the step (2), the using amount of the carbon dioxide is 10-15% of the mass of the enzymatic hydrolysis camellia seed meal.
Further, in the step (2), the microwave power is 700-.
The invention has the beneficial effects that:
according to the invention, the camellia seed meal is dried after being crushed, and impurities in the camellia seed meal are further removed, so that the material has large gaps and more space for contacting a solvent; the camellia seed meal is decomposed by mixing water and adding enzyme, so that the cell molecular structure of the camellia seed meal is dispersed, and the infiltration effect of a solvent is improved; then spray drying to evaporate water and keep the components of the material intact.
On the basis of the previous step, the invention expands the soluble target range by using the extraction solvent formed by mixing deionized water, absolute ethyl alcohol and ethyl acetate, is more beneficial to extracting the tea saponin combined with other water-soluble and alcohol-soluble substances, and can obviously improve the extraction rate of the tea saponin. Moreover, the content of carbonate in the mixed system is increased by the carbon dioxide with lower concentration, so that the metal ions in the camellia seed meal can be removed, the precipitation of components such as calcium, magnesium and the like is facilitated, and the refining efficiency of subsequent acid dissolution is enhanced; in addition, through twice microwave treatments, the extraction solvent and the camellia seed meal have better contact, the extraction solvent is promoted to permeate into cells of the camellia seed meal, and the tea saponin is maximally dissolved.
The method comprises the steps of mixing the crude tea saponin products, dissolving the residual lipid components by using benzene, further refining by using acetic acid, dissolving the tea saponin again, and removing the non-acid-soluble components in the tea saponin, so that the purity of the tea saponin is higher.
The extraction conditions are mild, and the extracted tea saponin is complete, so that the prepared tea saponin has higher activity and more purposes.
Detailed Description
Example 1
A method for purifying tea saponin comprises the following steps:
(1) oil tea seed meal treatment
Crushing camellia seed meal into 100-mesh powder, drying at 15 ℃ under 0.1 standard atmospheric pressure for 3 hours, mixing the powder with purified water 10 times of the mass of the powder, adjusting the ph of the mixed solution to 5.3 by using an acetic acid solution, adding cellulase 5% of the mass of the mixed solution, stirring at 40 ℃ at 80r/min for 50 minutes, adjusting the ph of the mixed solution to 8 by using a calcium hydroxide solution, adding protease 2% of the mass of the mixed solution, mixing at 53 ℃ at 100r/min for 30 minutes, spray-drying the mixed solution, and drying at 15 ℃ under 0.01 standard atmospheric pressure for 30 minutes to obtain enzymolysis camellia seed meal; the mass fraction of the acetic acid solution is 8%; the mass fraction of the calcium hydroxide solution is 0.3%;
(2) crude extraction of tea saponin
Mixing the enzymatic hydrolysis oil Camellia seed meal with extraction solvent, stirring at 20 deg.C for 5min at 300r/min, standing for 1h, introducing carbon dioxide, sealing, soaking at 30 deg.C for 30min, heating to 43 deg.C with microwave, keeping the temperature for 10min, naturally cooling the mixed system to room temperature, heating to 38 deg.C with microwave, keeping the temperature for 20min, and filtering; drying the filtrate under reduced pressure, mixing the obtained powder with n-butanol 10 times the weight of the powder at 40 deg.C, soaking for 20min, filtering, and drying the obtained filtrate under reduced pressure to obtain crude product of tea saponin; the extraction solvent is formed by mixing deionized water, absolute ethyl alcohol and ethyl acetate according to the mass ratio of 3:5: 1; the using amount of the carbon dioxide is 10% of the mass of the enzymolysis camellia seed meal; the microwave power is 700W;
(3) refining tea saponin crude product
Mixing the crude product of tea saponin with benzene 8 times of the weight of the crude product, stirring at high speed of 800r/min for 10min at 40 ℃, standing for 3h, filtering, and drying the filter residue under reduced pressure; mixing the obtained dry product with 10 times of acetic acid, standing for 30-50min, filtering, and drying under reduced pressure to obtain purified tea saponin.
Example 2
A method for purifying tea saponin comprises the following steps:
(1) oil tea seed meal treatment
Crushing camellia seed meal into 200-mesh powder, drying for 5 hours at 20 ℃ under 0.3 standard atmospheric pressure, mixing the powder with purified water 13 times of the mass of the powder, adjusting the ph of the mixed solution to 5.5 by using an acetic acid solution, adding cellulase 8% of the mass of the mixed solution, stirring for 80 minutes at 200r/min under 45 ℃, adjusting the ph of the mixed solution to 8.5 by using a calcium hydroxide solution, adding protease 3% of the mass of the mixed solution, mixing for 50 minutes at 150r/min under 55 ℃, spray-drying the mixed solution, and drying for 50 minutes at 20 ℃ under 0.03 standard atmospheric pressure to obtain enzymolysis camellia seed meal; the mass fraction of the acetic acid solution is 12%; the mass fraction of the calcium hydroxide solution is 0.5%;
(2) crude extraction of tea saponin
Mixing the enzymatic hydrolysis oil Camellia seed meal with an extraction solvent, stirring at 25 ℃ for 8min at a speed of 500r/min, standing for 3h, introducing carbon dioxide, sealing, soaking at 35 ℃ for 50min, heating to 45 ℃ with microwaves, preserving heat for 15min, naturally cooling the mixed system to room temperature, heating the mixed system to 43 ℃ with microwaves, preserving heat for 30min, and filtering; drying the filtrate under reduced pressure, mixing the obtained powder with n-butanol 20 times the weight of the powder at 45 deg.C, soaking for 30min, filtering, and drying the obtained filtrate under reduced pressure to obtain crude product of tea saponin; the extraction solvent is formed by mixing deionized water, absolute ethyl alcohol and ethyl acetate according to a mass ratio of 5:8: 2; the using amount of the carbon dioxide is 15% of the mass of the enzymolysis camellia seed meal; the microwave power is 800W;
(3) refining tea saponin crude product
Mixing the crude product of tea saponin with benzene 10 times of the weight of the crude product, stirring at high speed of 900r/min for 15min at 50 ℃, standing for 5h, filtering, and drying the filter residue under reduced pressure; mixing the obtained dry product with 20 times of acetic acid, standing for 50min, filtering, and drying under reduced pressure to obtain purified tea saponin.
Example 3
A method for purifying tea saponin comprises the following steps:
(1) oil tea seed meal treatment
Crushing camellia seed meal into 200-mesh powder, drying at 18 ℃ under 0.1 standard atmospheric pressure for 4 hours, mixing the powder with purified water 13 times of the mass of the powder, adjusting the ph of a mixed solution to 5.3 by using an acetic acid solution, adding cellulase 8% of the mass of the mixed solution, stirring at 40 ℃ at 200r/min for 50 minutes, adjusting the ph of the mixed solution to 8.5 by using a calcium hydroxide solution, adding protease 2% of the mass of the mixed solution, mixing at 55 ℃ at 100r/min for 50 minutes, spray-drying the mixed solution, and drying at 15 ℃ under 0.03 standard atmospheric pressure for 35 minutes to obtain enzymatic hydrolysis camellia seed meal; the mass fraction of the acetic acid solution is 11%; the mass fraction of the calcium hydroxide solution is 0.45%;
(2) crude extraction of tea saponin
Mixing the enzymatic hydrolysis oil Camellia seed meal with an extraction solvent, stirring at 23 deg.C for 7min at 400r/min, standing for 3h, introducing carbon dioxide, sealing, soaking at 30 deg.C for 50min, heating to 43 deg.C with microwave, keeping the temperature for 15min, naturally cooling the mixed system to room temperature, heating to 43 deg.C with microwave, keeping the temperature for 20min, and filtering; drying the filtrate under reduced pressure, mixing the obtained powder with n-butanol 20 times the weight of the powder at 40 deg.C, soaking for 30min, filtering, and drying the obtained filtrate under reduced pressure to obtain crude product of tea saponin; the extraction solvent is formed by mixing deionized water, absolute ethyl alcohol and ethyl acetate according to a mass ratio of 5:5: 1; the using amount of the carbon dioxide is 15% of the mass of the enzymolysis camellia seed meal; the microwave power is 700W;
(3) refining tea saponin crude product
Mixing the crude product of tea saponin with benzene 10 times of the weight of the crude product, stirring at high speed of 900r/min for 10min at 40 ℃, standing for 5h, filtering, and drying the filter residue under reduced pressure; mixing the obtained dry product with acetic acid 10 times of the dry product, standing for 50min, filtering, and drying under reduced pressure to obtain purified tea saponin.
To verify the effect of the invention, the following comparative examples were set up:
experimental examples the extraction rate and purity of tea saponin according to the present invention were tested (refer to the related technical standards and experimental methods, and the following schemes were designed).
1. 80g of camellia seed meal is weighed respectively, the steps are carried out according to examples 1-3 and comparative examples 1-9, and the obtained finished products are marked and weighed respectively to calculate the extraction rate.
2. Purity detection is measured by a vanillin-concentrated sulfuric acid method for calculating the mass fraction of saponin according to the saponin proportion, and the vanillin-concentrated sulfuric acid can react with the saponin to form a characteristic red color, so that the method is a widely adopted saponin color development method. The principle is that the saponin is a compound of tetracyclic or pentacyclic triterpene containing glycosidic bond, and hydroxyl groups on C3 and C12 can react with aldehyde group on vanillin to form acetal, so as to form a new conjugated system for color development. And (3) establishing a standard curve, namely accurately weighing 0.8g of vanillin, dissolving the vanillin in 10mL of absolute ethyl alcohol, and preparing a vanillin solution. 77 mL of concentrated sulfuric acid is taken and mixed with 23mL of deionized water for standby. Weighing 25mg of tea saponin standard substance, dissolving in a 50mL volumetric flask with 80% ethanol solution, fixing the volume, and shaking up to obtain the standard solution. Taking 0.5mL of standard solution, accurately adding 0.5mL of 80g/L vanillin solution, adding 4mL of 77% sulfuric acid solution into ice water, shaking up, heating at 60 ℃ for 15min, then placing in an ice water bath for cooling for 10min, taking out, placing at room temperature, taking a reagent as a blank, and scanning on an ultraviolet-visible spectrophotometer by using a 1cm cuvette to obtain the maximum absorption wavelength. Taking 0.1 mL, 0.2 mL, 0.3 mL, 0.4 mL, 0.5mL and 0.6mL of the tea saponin standard solution, placing the solution in a test tube with a plug, adding water to fix the volume to 1mL, adding the reagent according to the method for reaction, measuring the absorbance under the maximum absorption wavelength, drawing a standard curve by using the absorbance to the concentration value, and establishing a regression equation.
Weighing about 65.0mg of each group of tea saponin respectively, metering to 25mL with 80% ethanol, taking 1mL to measure absorbance, adding into corresponding regression equation, and calculating saponin mass fraction according to standard curve.
3. Preparing each group of tea saponin into 10mL of 5mg/mL solution, picking 3-4 loops of activated and cultured escherichia coli for about 48 hours by using an inoculating loop, and preparing the escherichia coli into bacterial suspension with proper concentration in 150mL of sterile nutrient broth liquid culture medium. And pouring the nutrient broth agar culture medium cooled to about 50 ℃ into a sterilized culture dish, cooling, dripping 100 mu L of bacterial suspension, and uniformly coating the bacterial suspension by using a sterilization coater to obtain the bacterial-containing flat plate. After no flowing liquid exists on the surface of the bacteria-containing flat plate, 3 sterilized Oxford cups are stably and equidistantly placed in each culture dish, 20 mu L of prepared tea saponin solution is dripped into the Oxford cups in sequence, and sterile normal saline is dripped into the 3 rd Oxford cup to serve as blank control. Transferring into a constant temperature incubator at 37 ℃ for 3d, observing the growth condition of each strain, and measuring the diameter of each inhibition zone according to the vertical direction.
The experimental results are as follows:
| extraction rate | Saponin mass fraction | Bacteriostatic diameter | |
| Example 1 | 86.75％ | 91.27％ | 13.8 |
| Example 2 | 85.89％ | 93.74％ | 13.2 |
| Example 3 | 85.16％ | 92.46％ | 13.7 |
| Comparative example 1 | 80.29％ | 85.69％ | 13.1 |
| Comparative example 2 | 81.12％ | 86.91％ | 12.5 |
| Comparative example 3 | 81.81％ | 86.71％ | 12.3 |
| Comparative example 4 | 76.51％ | 81.23％ | 11.6 |
| Comparative example 5 | 75.34％ | 80.59％ | 12.2 |
| Comparative example 6 | 82.78％ | 84.22％ | 11.9 |
| Comparative example 7 | 82.70％ | 81.79％ | 11.3 |
| Comparative example 8 | 83.59％ | 83.85％ | 13.9 |
| Comparative example 9 | 82.10％ | 84.35％ | 12.3 |
| Comparative example 10 | 81.70％ | 85.13％ | 11.5 |
It can be seen that the tea saponin prepared by the method has high extraction rate, high saponin mass fraction and significantly better antibacterial effect than the comparative examples 1-10, so the method effectively ensures the activity of the tea saponin during extraction.
Claims (6)
1. The method for purifying tea saponin is characterized by comprising the following steps:
(1) oil tea seed meal treatment
Crushing the camellia seed meal into powder of 100-plus 200 meshes, drying for 3-5h at 15-20 ℃ under 0.1-0.3 standard atmospheric pressure, mixing the powder with purified water of which the mass is 10-13 times of that of the powder, adjusting the ph of the mixed solution to 5.3-5.5 by using an acetic acid solution, adding cellulase of which the mass is 5-8% of that of the mixed solution, stirring for 50-80min at 40-45 ℃ at 80-200r/min, adjusting the ph of the mixed solution to 8-8.5 by using a calcium hydroxide solution, adding protease of which the mass is 2-3% of that of the mixed solution, stirring for 30-50min at 53-55 ℃ at 100-150r/min, spray-drying the mixed solution, and drying for 30-50min at 15-20 ℃ under 0.01-0.03 standard atmospheric pressure to obtain the enzymolysis camellia seed meal;
(2) crude extraction of tea saponin
Mixing the enzymatic hydrolysis camellia seed meal with an extraction solvent, stirring for 5-8min at 20-25 ℃ at 500r/min, standing for 1-3h, introducing carbon dioxide, sealing, soaking at 30-35 ℃ for 30-50min, heating to 43-45 ℃ by microwave, preserving heat for 10-15min, naturally cooling the mixed system to room temperature, heating to 38-43 ℃ by microwave, preserving heat for 20-30min, and filtering; drying the filtrate under reduced pressure, mixing the obtained powder with n-butanol 10-20 times the weight of the powder at 40-45 deg.C, soaking for 20-30min, filtering, and drying the filtrate under reduced pressure to obtain crude product of tea saponin;
(3) refining tea saponin crude product
Mixing the crude product of tea saponin with benzene 8-10 times of the mass of the crude product, stirring at high speed of 900r/min at 40-50 ℃ for 10-15min, standing for 3-5h, filtering, and drying the filter residue under reduced pressure; mixing the obtained dry product with 10-20 times of acetic acid, standing for 30-50min, filtering, and drying under reduced pressure to obtain purified tea saponin.
2. The method for purifying tea saponin according to claim 1, wherein in the step (1), the mass fraction of the acetic acid solution is 8-12%.
3. The method for purifying tea saponin according to claim 1, wherein in the step (1), the mass fraction of the calcium hydroxide solution is 0.3-0.5%.
4. The method for purifying tea saponin according to claim 1, wherein in the step (2), the extraction solvent is formed by mixing deionized water, absolute ethyl alcohol and ethyl acetate in a mass ratio of 3-5:5-8: 1-2.
5. The method for purifying tea saponin according to claim 1, wherein in the step (2), the amount of the carbon dioxide is 10-15% of the mass of the enzymatic hydrolysis camellia seed meal.
6. The method for purifying tea saponin as claimed in claim 1, wherein in the step (2), the microwave power is 700-800W.
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