CN116396351A - Tea dreg processing method - Google Patents
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- 238000003672 processing method Methods 0.000 title claims abstract description 8
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 270
- 241001122767 Theaceae Species 0.000 claims abstract description 192
- 239000001397 quillaja saponaria molina bark Substances 0.000 claims abstract description 97
- 229930182490 saponin Natural products 0.000 claims abstract description 97
- 150000007949 saponins Chemical class 0.000 claims abstract description 97
- 238000002386 leaching Methods 0.000 claims abstract description 81
- 235000012054 meals Nutrition 0.000 claims abstract description 49
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 48
- 238000000034 method Methods 0.000 claims abstract description 32
- 239000006228 supernatant Substances 0.000 claims abstract description 26
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000012360 testing method Methods 0.000 claims abstract description 20
- 238000001035 drying Methods 0.000 claims abstract description 15
- 239000003208 petroleum Substances 0.000 claims abstract description 11
- 238000000926 separation method Methods 0.000 claims abstract description 6
- 238000005238 degreasing Methods 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 61
- 238000012545 processing Methods 0.000 claims description 9
- 238000004364 calculation method Methods 0.000 claims description 8
- 238000002835 absorbance Methods 0.000 claims description 6
- 238000010790 dilution Methods 0.000 claims description 3
- 239000012895 dilution Substances 0.000 claims description 3
- 238000000605 extraction Methods 0.000 abstract description 44
- 238000002137 ultrasound extraction Methods 0.000 abstract description 12
- 230000004044 response Effects 0.000 abstract description 10
- 235000013616 tea Nutrition 0.000 description 145
- 230000000694 effects Effects 0.000 description 10
- 239000002904 solvent Substances 0.000 description 9
- 238000005303 weighing Methods 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 235000019441 ethanol Nutrition 0.000 description 5
- 238000003809 water extraction Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000013461 design Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000000194 supercritical-fluid extraction Methods 0.000 description 3
- 241000209507 Camellia Species 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
- 239000010495 camellia oil Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 235000018597 common camellia Nutrition 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000000611 regression analysis Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- MWOOGOJBHIARFG-UHFFFAOYSA-N vanillin Chemical compound COC1=CC(C=O)=CC=C1O MWOOGOJBHIARFG-UHFFFAOYSA-N 0.000 description 2
- FGQOOHJZONJGDT-UHFFFAOYSA-N vanillin Natural products COC1=CC(O)=CC(C=O)=C1 FGQOOHJZONJGDT-UHFFFAOYSA-N 0.000 description 2
- 235000012141 vanillin Nutrition 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 238000000540 analysis of variance Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
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- 230000007423 decrease Effects 0.000 description 1
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- 238000011161 development Methods 0.000 description 1
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- 238000004090 dissolution Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000013401 experimental design Methods 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
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- 239000007787 solid Substances 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 238000005211 surface analysis Methods 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 235000020338 yellow tea Nutrition 0.000 description 1
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- 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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- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
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Abstract
The invention discloses a processing method of tea seed cake, which comprises the following steps: preparing a small amount of tea meal, washing and crushing; drying the crushed tea seed cake, degreasing the tea seed cake by petroleum ether, and preparing defatted tea seed cake; dissolving a proper amount of defatted tea meal in a methanol solution; ultrasonic leaching or water bath leaching is carried out on defatted tea meal obtained by dissolving in methanol solution; centrifugal separation is carried out on defatted tea meal after ultrasonic leaching or water bath leaching to obtain supernatant; concentrating and drying the obtained supernatant to constant weight to obtain tea saponin; the method is characterized in that the ultrasonic-assisted methanol is adopted to extract tea saponin, and a response surface method is applied to an extraction process of the tea saponin in tea seed meal on the basis of a single factor test; the three methods of water bath extraction, ultrasonic extraction and water bath extraction are compared to obtain the tea saponin with the highest yield obtained by ultrasonic extraction and water bath extraction, and compared with the prior art, the tea saponin prepared under the optimal conditions has the highest yield and purity.
Description
Technical Field
The invention relates to the technical field of tea dreg processing, in particular to a tea dreg processing method.
Background
The tea seed resources in China are quite rich, about 100 ten thousand tons of tea-oil camellia meal are available, and 30 ten thousand tons of tea saponin can be produced by annual conservative calculation if the tea-oil camellia meal is fully utilized; however, the actual utilization rate is only about 10%, most tea cakes are not exported to abroad, and the fertilizer is burnt inappropriately, so that the resources are wasted, the environment is destroyed, the tea cakes are harmless, and the most critical problem is how to effectively utilize the tea cakes.
In the prior art, the extraction process of tea saponin comprises the following steps: water extraction, alcohol extraction, supercritical extraction, flash extraction, ultrasonic assisted, microwave assisted, alcohol extraction, etc.; wherein, the water extraction method is long in time consumption, and the extracting solution is not easy to store, mold and deteriorate; the alcohol extraction method has the advantages of less solvent, low boiling point, difficult mildew, easy recovery of the solvent, less water-soluble impurities in the leaching solution and the like, and is commonly used in industry; the supercritical extraction method has the characteristics of high efficiency, cleanness, no pollution and the like, and has wider application range, but the extraction process is carried out under high pressure, so the requirements on equipment investment and operation cost are higher, and the investment is larger; the flash extraction method has high extraction efficiency, saves time (only 30S is needed for one extraction), is simple and convenient to operate, and is beneficial to environmental protection; the ultrasonic auxiliary method has the advantages of short extraction time, high efficiency, mild conditions and the like, and can effectively avoid the damage of high temperature and high pressure to the extracted components; the disadvantage of the microwave-assisted method is that the solvents used must be polar, since only polar substances absorb microwave energy, the method is also somewhat limited in its application; the alcohol extraction method has the advantages of short extraction time, mild conditions, high extraction rate, environmental protection and the like;
based on the above, the water extraction method has more defects, so that the water extraction method is not suitable for extracting tea seed meal, and the supercritical extraction method has the advantages of high efficiency and cleanness, but has large investment and is also unsuitable; the microwave assisted method has a limitation because the solvent must be polar, and the alcohol extraction method, the ultrasonic assisted method and the flash extraction method have certain advantages and have no obvious defects, so a tea seed cake treatment method is proposed to solve the above problems.
Disclosure of Invention
In order to overcome the defects in the prior art and solve the problems, the invention provides a tea seed cake processing method.
A method for treating tea seed cake, comprising the steps of:
s1: preparing a small amount of tea meal, washing and crushing;
s2: drying the crushed tea seed cake, degreasing the tea seed cake by petroleum ether, and preparing defatted tea seed cake;
s3: dissolving a proper amount of defatted tea meal in a methanol solution;
s4: ultrasonic leaching or water bath leaching is carried out on defatted tea meal obtained by dissolving in methanol solution;
s5: centrifugal separation is carried out on defatted tea meal after ultrasonic leaching or water bath leaching to obtain supernatant;
s6: concentrating and drying the obtained supernatant to constant weight to obtain tea saponin;
s7: testing purity and yield of tea saponin;
repeating the steps S3-S7, dissolving the defatted tea seed meal with methanol solutions with different volumes and the same volume fraction, and determining the methanol solution with the optimal volume; dissolving defatted tea meal with the same weight in methanol solutions with the same volume and different volume fractions; an optimal volume fraction of the methanol solution is determined.
Preferably, in the step S4, the defatted tea seed cake is treated by ultrasonic leaching, and in order to determine the optimal ultrasonic time, the defatted tea seed cake with the same weight is taken and dissolved in a methanol solution with the optimal volume and the optimal volume fraction; setting the same ultrasonic frequency, and treating the defatted tea meal dissolved in the methanol solution at different ultrasonic times; repeating steps S5 to S7, and determining the optimal ultrasonic time.
Preferably, in the step S4, the defatted tea seed cake is treated by ultrasonic leaching, and in order to determine the optimal ultrasonic frequency, the defatted tea seed cake with the same weight is taken and dissolved in a methanol solution with the optimal volume and the optimal volume fraction; setting the same ultrasonic time, and treating the defatted tea meal dissolved in the methanol solution at different ultrasonic frequencies; repeating steps S5 to S7, and determining the optimal ultrasonic frequency.
Preferably, in the step S4, the defatted tea seed cake is leached in a water bath, and in order to determine the optimal leaching time, the defatted tea seed cake with the same weight is taken and dissolved in a methanol solution with the optimal volume and the optimal volume fraction; leaching in water bath with the same temperature for different time; repeating steps S5 to S7, and determining the optimal leaching time.
Preferably, in the step S4, the defatted tea seed cake is leached in a water bath, and in order to determine the optimal leaching temperature, the defatted tea seed cake with the same weight is taken and dissolved in a methanol solution with the optimal volume and the optimal volume fraction; controlling the same water bath leaching time and controlling different leaching temperatures; steps S5 to S7 are repeated to determine the optimal leaching temperature.
Preferably, in the step S6, the supernatant is concentrated and dried to a constant weight, and the supernatant is concentrated to a paste state at a vacuum degree of 0.09Mpa and a temperature of 55 ℃, and then dried to a constant weight.
Preferably, in the step S7, the calculation formula of the purity and yield of the tea saponin is as follows:
tea saponin purity = (a-0.0626) ×v×n/8.0918×m 1 *100％；
Tea saponin yield = tea saponin purity M 2 /M 3 *100％；
Wherein:
a is absorbance; v is the volume ml of the solution; n is the multiple of the dilution of the solution; m is M 1 is Measuring the amount mg of the tea saponin weighed by the A; m is M 2 The amount of tea saponin is mg; m is M 3 Is the weight of the defatted tea seed cake.
Preferably, in the step S4, at least one of ultrasonic leaching and water bath leaching is used, and the tea saponin can also be extracted by matching ultrasonic leaching with water bath leaching.
The invention has the advantages that:
the invention adopts ultrasonic-assisted methanol to extract tea saponin, and applies a response surface method to the extraction process of tea saponin in tea seed meal on the basis of a single factor test. The results show that: the leaching temperature and the methanol addition have remarkable influence on the tea saponin yield, and the influence degree is expressed as that the leaching temperature is greater than the methanol addition and the methanol volume fraction. Taking defatted tea seed meal as a raw material, and under the optimal process conditions: the methanol addition amount is 45mL, the methanol volume fraction is 83%, the ultrasonic time is 30min, the ultrasonic frequency is 25.97kHz, the leaching time is lh, the leaching temperature is 56 ℃, and the pale yellow tea saponin with the purity of 85% and the yield of 24.16% can be obtained after drying.
The method is characterized in that three methods of water bath extraction, ultrasonic and water bath extraction are compared to obtain the highest yield of the tea saponin obtained by ultrasonic and water bath extraction, and the method is the optimal method for extracting the tea saponin.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions of the prior art, the drawings which are used in the description of the embodiments or the prior art will be briefly described, it being obvious that the drawings in the description below are only some embodiments of the invention, and that other drawings can be obtained from these drawings without inventive faculty for a person skilled in the art.
FIG. 1 is a flow chart of a processing method according to an embodiment of the present invention;
FIG. 2 is a graph showing the effect of methanol addition on tea saponin yield in one embodiment of the present invention;
FIG. 3 is a graph showing the effect of methanol volume fraction on tea saponin yield in one embodiment of the present invention;
FIG. 4 is a graph showing the effect of ultrasonic time on tea saponin yield in one embodiment of the present invention;
FIG. 5 is a graph showing the effect of ultrasonic frequency on tea saponin yield in one embodiment of the present invention;
FIG. 6 is a graph showing the effect of extraction time on tea saponin yield in one embodiment of the present invention;
FIG. 7 is a graph showing the effect of extraction temperature on tea saponin yield in one embodiment of the present invention;
FIG. 8 is a graph showing comparison of the yields of tea saponin extracted by ultrasonic leaching, water bath leaching and ultrasonic-combined water bath in one embodiment of the present invention;
FIG. 9 is a response surface plot of methanol volume fraction, methanol addition in one embodiment of the invention;
FIG. 10 is a graph showing the response of methanol volume fraction and leaching temperature in one embodiment of the present invention;
FIG. 11 is a graph showing the response of methanol addition and leaching temperature in one embodiment of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Referring to fig. 1-11, a method for processing tea seed cake includes the following steps:
s1: preparing a small amount of tea meal, washing and crushing;
s2: drying the crushed tea seed cake, degreasing the tea seed cake by petroleum ether, and preparing defatted tea seed cake;
s3: dissolving a proper amount of defatted tea meal in a methanol solution;
s4: ultrasonic leaching or water bath leaching is carried out on defatted tea meal obtained by dissolving in methanol solution;
s5: centrifugal separation is carried out on defatted tea meal after ultrasonic leaching or water bath leaching to obtain supernatant;
s6: concentrating and drying the obtained supernatant to constant weight to obtain tea saponin;
s7: testing purity and yield of tea saponin;
repeating the steps S3-S7, dissolving the defatted tea seed meal with methanol solutions with different volumes and the same volume fraction, and determining the methanol solution with the optimal volume; dissolving defatted tea meal with the same weight in methanol solutions with the same volume and different volume fractions; an optimal volume fraction of the methanol solution is determined.
Specifically, an optimal volume of methanol solution is determined, specifically:
weighing 6 parts of petroleum ether defatted tea seed meal, dissolving 5g of each in 70% methanol solution, respectively adding 30, 35, 40, 45, 50 and 55mL of methanol solution, carrying out water bath extraction for 2 hours at 60 ℃ after ultrasonic frequency is 25.97kHz and ultrasonic time is 20min, centrifuging to obtain supernatant, concentrating the supernatant into paste at the vacuum degree of 0.09Mpa and the temperature of 55 ℃, drying the paste to constant weight, and calculating the tea saponin yield; calculated, 55ml of methanol solution is added, and the tea saponin yield is highest;
as shown in figure 2, the tea saponin yield increases sharply with increasing methanol addition, and the tea saponin yield does not change basically when the methanol addition reaches 45 ml;
the optimal volume fraction of the methanol solution is determined, specifically:
weighing 6 parts of petroleum ether defatted tea seed meal, adding 5g of each of the petroleum ether defatted tea seed meal into 55mL of methanol solution, respectively preparing 65%, 70%, 75%, 80%, 85% and 90% of methanol solution, carrying out ultrasonic extraction for 2 hours in a water bath at 60 ℃ after ultrasonic frequency is 25.97kHz and ultrasonic time is 20min, centrifuging to obtain supernatant, concentrating the supernatant to paste at the vacuum degree of 0.09Mpa and the temperature of 55 ℃, drying the paste to constant weight, and calculating the tea saponin yield; the calculation shows that the yield of the tea saponin is highest in 80% methanol solution;
as shown in figure 3, the different methanol volume fractions have different influences on the tea saponin yield, and the tea saponin yield is highest when methanol with the volume fraction of 80% is used as the leaching agent. The analysis reason is that when the methanol is lower, the water-soluble impurities in the extracted leaching solution are more, so that the extraction amount of tea saponin is less; however, at concentrations above 80%, the yield begins to drop because tea saponin is readily soluble in aqueous methanol, but not in nearly anhydrous methanol solvents; and the higher the methanol concentration; and the higher the concentration of methanol, the more volatile it is, and the more lost it is, so the most suitable is 80% of the leaching agent methanol.
In S4, the defatted tea seed cake is treated by ultrasonic leaching, and in order to determine the optimal ultrasonic time, the same weight of defatted tea seed cake is taken and dissolved in a methanol solution with optimal volume and optimal volume fraction; setting the same ultrasonic frequency, and treating the defatted tea meal dissolved in the methanol solution at different ultrasonic times; repeating the steps S5 to S7, and determining the optimal ultrasonic time;
specifically, the optimal ultrasonic time is determined, specifically:
weighing 6 parts of petroleum ether defatted tea seed meal, adding 55mL of 80% methanol solution into each 5g, respectively setting ultrasonic time to be 15, 20, 25, 30, 35 and 40min at ultrasonic frequency of 25.97kHz, leaching for 2h in a water bath at 60 ℃, centrifugally separating to obtain supernatant, concentrating the supernatant to paste at vacuum degree of 0.09Mpa and temperature of 55 ℃, drying the paste to constant weight, and calculating the tea saponin yield; the tea saponin yield is highest when the ultrasonic time is 30 min;
as shown in figure 4, the tea saponin yield increases with the ultrasonic time, and decreases after rising, and when the ultrasonic time reaches 30min, the tea saponin yield is highest. Because the vibration of ultrasonic wave makes tea saponin dissolve fast, but along with the extension of time, the ultrasonic wave heat can destroy the structure of tea saponin again for tea saponin yield drops, so the ultrasonic time of 30min is preferred.
In S4, the defatted tea seed cake is treated by ultrasonic leaching, and in order to determine the optimal ultrasonic frequency, the same weight of defatted tea seed cake is taken and dissolved in a methanol solution with optimal volume and optimal volume fraction; setting the same ultrasonic time, and treating the defatted tea meal dissolved in the methanol solution at different ultrasonic frequencies; repeating steps S5 to S7, and determining the optimal ultrasonic frequency.
Specifically, the optimal ultrasonic frequency is determined, specifically:
weighing 6 parts of petroleum ether defatted tea seed meal, adding 55mL of 80% methanol solution into each 5g, respectively performing ultrasonic extraction for 30min at ultrasonic frequencies of 0.5kHz, 14.65kHz, 25.97kHz and 34.51kHz, then performing water bath extraction for 2h at 60 ℃, performing centrifugal separation to obtain supernatant, concentrating the supernatant into paste at a vacuum degree of 0.09Mpa and a temperature of 55 ℃, drying the paste to constant weight, and calculating the tea saponin yield; the tea saponin yield is highest when the ultrasonic frequency is 25.97 kHz;
as shown in figure 5, under the condition of no ultrasonic treatment, the tea saponin yield is very low, and with the increase of ultrasonic frequency, the tea saponin yield shows the development trend of increasing and decreasing, and at the ultrasonic frequency of 25.97kHz, the tea saponin yield reaches the maximum. This is because the ultrasonic wave has the greatest effect when the ultrasonic frequency matches the vibration frequency generated by the solid particles in the extraction liquid, and therefore the ultrasonic frequency is preferably 25.97 kHz.
In S4, the defatted tea seed cake is leached in a water bath, and in order to determine the optimal leaching time, the same weight of defatted tea seed cake is taken and dissolved in a methanol solution with optimal volume and optimal volume fraction; leaching in water bath with the same temperature for different time; repeating steps S5 to S7, and determining the optimal leaching time.
Specifically, the optimal leaching time is determined, specifically:
weighing 6 parts of petroleum ether defatted tea seed cake, adding 55mL of 80% methanol solution, performing ultrasonic extraction for 30min at an ultrasonic frequency of 25.97kHz, respectively setting the extraction time in a water bath at 60 ℃ to be 0, 1, 2, 3, 4 and 5 hours, performing centrifugal separation to obtain supernatant, concentrating the supernatant to paste at a vacuum degree of 0.09Mpa and a temperature of 55 ℃, drying the paste to constant weight, and calculating the tea saponin yield; the tea saponin with the leaching time of 1h is obtained by calculation, and the yield is highest;
as shown in figure 6, the leaching time is from 0 to 1h, the tea saponin yield rises faster, and then the curve is gentle and has no larger fluctuation along with the extension of time, and the leaching time is preferably 1h in consideration of the fact that the energy consumption is increased and the color of the leaching solution is deepened along with the extension of the leaching time.
In S4, the defatted tea seed cake is leached in a water bath, and in order to determine the optimal leaching temperature, the same weight of defatted tea seed cake is taken and dissolved in a methanol solution with optimal volume and optimal volume fraction; controlling the same water bath leaching time and controlling different leaching temperatures; repeating steps S5 to S7, and determining the optimal leaching temperature;
specifically, the optimal leaching temperature is determined, specifically:
weighing 6 parts of petroleum ether defatted tea seed cake, adding 55mL of 80% methanol solution, performing ultrasonic extraction for 30min at an ultrasonic frequency of 25.97kHz, respectively extracting at water bath temperatures of 25, 35, 45, 55, 65 and 75 ℃ for 1h, centrifuging to obtain supernatant, concentrating the supernatant to paste at a vacuum degree of 0.09Mpa and a temperature of 55 ℃, drying the paste to constant weight, and calculating the tea saponin yield; the tea saponin yield is highest when the leaching temperature is 55 ℃ through calculation;
as shown in figure 7, the tea saponin yield is highest when the leaching temperature is 55 ℃. Then, the yield of the tea saponin is reduced due to the increase of the temperature, and the tea saponin yield is reduced probably due to the reaction of impurities extracted from the tea seed meal and the tea saponin at high temperature. Therefore, the leaching temperature is suitably 55 ℃.
In one embodiment of the invention, in S6, the supernatant is concentrated and dried to a constant weight, and the supernatant is concentrated to a paste state at a temperature of 55 ℃ under a vacuum degree of 0.09Mpa and then dried to a constant weight.
In S7, the calculation formula of the purity and yield of the tea saponin is as follows:
tea saponin purity = (a-0.0626) ×v×n/8.0918×m 1 *100％；
Tea saponin yield = tea saponin purity M 2 /M 3 *100％；
Wherein:
a is absorbance; v is the volume ml of the solution; n is the multiple of the dilution of the solution; m is M 1 is Measuring the amount mg of the tea saponin weighed by the A; m is M 2 The amount of tea saponin is mg; m is M 3 Is the weight of the defatted tea seed cake.
Specifically, the absorbance A of the prepared tea saponin is specifically: accurately weighing 0.0083g of crude tea saponin, dissolving in 70% methanol, fixing volume in 10ml volumetric flask, shaking uniformly, and collecting the solution0.3ml of the solution was aspirated and made up to 0.5ml with solvent, absorbance a was measured at 550nm λmax, and the measured a was substituted into regression equation a=0.0626+8.0918 c (R 2 =0.989), the purity and yield of crude tea saponin can be obtained;
specifically, the determination of λmax is specifically: precisely weighing 41.4mg of tea saponin standard substance dried to constant weight, dissolving with 70% methanol, fixing the volume to a 50ML volumetric flask, shaking uniformly, sucking 0.2ML of the standard solution into a test tube, adding 0.3ML of solvent (70% methanol), sucking 5ML of the now prepared 8% vanillin solution (2.0 g vanillin and a certain amount of absolute ethyl alcohol are dissolved, fixing the volume to a 25ML volumetric flask), sucking 4ML of 77% concentrated sulfuric acid under an ice bath environment, shaking uniformly, reacting the test tube in a water bath at 60 ℃ for 18min, then placing the test tube in an ice bath for 10min, taking out the test tube to return to room temperature, and measuring absorbance A at 480-600nm by using reagent blank as a reference to obtain a lambda max of 550nm;
in order to determine the influence of the leaching temperature, the methanol addition and the methanol volume fraction on the yield of the extracted tea saponin, a three-factor three-level test is designed, the influence of the methanol volume fraction, the methanol addition and the leaching temperature on the yield of the tea saponin is mainly investigated, and data fitting is carried out by using DsingExpert 8.0.7.1 software to optimize the extraction process parameters; the factors and level codes tested are shown in table 1 below:
table 1 test factor level
By X 1 ＝(A-80)/50，X 2 ＝(B-45)/5，X 3 The response surface analysis was performed with the tea saponin yield as the response value (Y) with = (C-55)/5 as the argument, and the experimental design and results of the center combination design are shown in table 2:
performing multiple fitting regression on the data in the table 2, and establishing a regression equation:
Y＝700.12113+3.95558X 1 +9.23793X 2 +12.38261X 3 —0.017396X l X 2 —6.41014E-003X l X 3 +O.088320X 2 X 3 -0.016813X 1 2 -0.13811X 2 2 -0.14192X 3 2
performing analysis of variance on the regression model obtained from the test data in Table 2, and the analysis results are shown in Table 3;
TABLE 3 regression analysis results
| Variance source | Degree of freedom | Sum of squares | Mean square sum | F value | Pr>F |
| Model | 9 | 133.72 | 14.86 | 42.21 | 0.0003 |
| X 1 | 1 | 3.39 | 3.39 | 9.62 | 0.0268 |
| X 2 | 1 | 15.06 | 15.06 | 42.78 | 0.0013 |
| X 3 | 1 | 10.86 | 10.86 | 30.86 | 0.0026 |
| X 1 X 2 | 1 | 0.76 | 0.76 | 2.15 | 0.2025 |
| X 1 X 3 | 1 | 0.10 | 0.10 | 0.29 | 0.6122 |
| X 2 X 3 | 1 | 19.50 | 19.50 | 55.40 | 0.007 |
| X 1 2 | 1 | 0.65 | 0.65 | 1.85 | 0.2315 |
| X 2 2 | 1 | 44.01 | 44.01 | 125.05 | <0.0001 |
| X 3 2 | 1 | 46.48 | 46.48 | 132.05 | <0.0001 |
| |
5 | 1.76 | 0.35 | ||
| |
3 | 0.90 | 0.30 | 0.69 | 0.6373 |
| |
2 | 0.86 | 0.43 | ||
| |
14 | 135.48 |
R 2 ＝0.9870；R adj 2 ＝0.9636；
The correlation coefficient R of the model can be obtained by variance analysis of the regression model 2 0.9870, the predicted values of the test have better consistency; r is R adj 2 0.9636, it shows that the model has good fitting degree and small test error, and the model is reasonable; the coefficient of variation cv=2.92, a lower CV value indicates a better reliability of the test, so that the regression equation can be used to analyze and predict the test result instead of the test true point. As can also be seen from further examination of the variances of the regression equations, X 2 、X 3 、X 2 X 3 、X 2 2 And X 3 2 The effect is remarkable. According to coefficient value x l ＝3.95558，X 2 ＝9.23793，X 3 The main effect relationship of = 12.38261, the factors are: leaching temperature>Methanol addition>Methanol volume fraction;
performing quadratic multiple regression fitting on the data, wherein the obtained quadratic response curved surface is shown in figures 9-11; the response surface and contour plots were made with the volume fraction of methanol, the methanol addition amount, and the leaching temperature at zero level, respectively, as shown in the above-mentioned FIGS. 9 to 11, it was found that the methanol addition amount (X 2 ) And leaching temperature (X) 3 ) Has obvious influence on the tea saponin yield, is shown by steeper curve, and has a methanol volume fraction (X 1 ) Since the curve is smoother, the effect on the extraction is less, which is consistent with the results of the regression analysis.
The test parameters are further optimized by the design expert8.0.7.1 software, so that the purpose of extracting more tea saponin is achieved, and the preferable conditions can be obtained as follows: the volume fraction of the methanol is 83.05%, the adding amount of the methanol is 45.16mL, the leaching temperature is 56.11 ℃, and under the condition, the tea saponin yield can reach 24.75%. In order to verify the reliability of the result obtained by the design, the test is verified, the tea saponin yield is measured by adopting the optimized process parameters, and under the optimal condition (the parameters are adjusted to 83% of methanol volume fraction, the methanol addition amount is 45mL, the leaching temperature is 56 ℃), the tea saponin yield is 24.16%, the purity is 85%, and compared with the theoretical value, the deviation is small. Therefore, the extraction condition parameters obtained by optimization by adopting the response surface method are accurate and reliable; compared with the prior art, the tea saponin prepared under the optimal condition has improved yield and purity.
In the step S4, at least one of ultrasonic extraction and water bath extraction is used, and the tea saponin may be extracted by ultrasonic extraction and water bath extraction.
In order to determine the optimal tea saponin extraction mode, weighing 5g of tea seed meal, extracting tea saponin by a water bath extraction method, an ultrasonic method, a water bath extraction method and the like, under the condition that the test conditions are the same, carrying out content measurement according to a tea saponin purity and yield calculation formula, carrying out parallel measurement for three times, recording data, and sequentially obtaining the tea saponin extracted by the three methods, wherein the yield is as follows: water bath + ultrasound > water bath. The reason is that in ultrasonic extraction, the strong vibration action can promote the cell rupture in plant tissue, the solvent permeates into the plant cell, so that the effective components in the cell enter the solvent to accelerate the mutual permeation and dissolution, and the extraction yield is much higher than that of water bath extraction; and the ultrasonic extraction alone can lead to incomplete extraction of the tea saponin, so the water bath extraction after the ultrasonic extraction leads to more sufficient extraction of the tea saponin, and the yield is increased. Therefore, the water bath extraction mode is optimal after the ultrasonic extraction is selected.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing has shown and described the basic principles, principal features and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims.
Claims (8)
1. A processing method of tea seed cake is characterized in that: the processing method comprises the following steps:
s1: preparing a small amount of tea meal, washing and crushing;
s2: drying the crushed tea seed cake, degreasing the tea seed cake by petroleum ether, and preparing defatted tea seed cake;
s3: dissolving a proper amount of defatted tea meal in a methanol solution;
s4: ultrasonic leaching or water bath leaching is carried out on defatted tea meal obtained by dissolving in methanol solution;
s5: centrifugal separation is carried out on defatted tea meal after ultrasonic leaching or water bath leaching to obtain supernatant;
s6: concentrating and drying the obtained supernatant to constant weight to obtain tea saponin;
s7: testing purity and yield of tea saponin;
repeating the steps S3-S7, dissolving the defatted tea seed meal with methanol solutions with different volumes and the same volume fraction, and determining the methanol solution with the optimal volume; dissolving defatted tea meal with the same weight in methanol solutions with the same volume and different volume fractions; an optimal volume fraction of the methanol solution is determined.
2. A method of processing tea seed cake according to claim 1, wherein: in the step S4, the defatted tea meal is treated by ultrasonic leaching, and in order to determine the optimal ultrasonic time, the defatted tea meal with the same weight is taken and dissolved in a methanol solution with the optimal volume and the optimal volume fraction; setting the same ultrasonic frequency, and treating the defatted tea meal dissolved in the methanol solution at different ultrasonic times; repeating steps S5 to S7, and determining the optimal ultrasonic time.
3. A method of processing tea seed cake according to claim 2, wherein: in the step S4, the defatted tea meal is treated by ultrasonic leaching, and in order to determine the optimal ultrasonic frequency, the defatted tea meal with the same weight is taken and dissolved in a methanol solution with the optimal volume and the optimal volume fraction; setting the same ultrasonic time, and treating the defatted tea meal dissolved in the methanol solution at different ultrasonic frequencies; repeating steps S5 to S7, and determining the optimal ultrasonic frequency.
4. A method of processing tea seed cake according to claim 3, wherein: in the step S4, the defatted tea meal is leached in a water bath, and in order to determine the optimal leaching time, the defatted tea meal with the same weight is taken and dissolved in a methanol solution with the optimal volume and the optimal volume fraction; leaching in water bath with the same temperature for different time; repeating steps S5 to S7, and determining the optimal leaching time.
5. A method of processing tea seed cake according to claim 4, wherein: in the step S4, the defatted tea meal is leached in a water bath, and in order to determine the optimal leaching temperature, the defatted tea meal with the same weight is taken and dissolved in a methanol solution with the optimal volume and the optimal volume fraction; controlling the same water bath leaching time and controlling different leaching temperatures; steps S5 to S7 are repeated to determine the optimal leaching temperature.
6. A method of processing tea seed cake according to claim 5, wherein: in the step S6, the supernatant is concentrated and dried to constant weight, and the supernatant is concentrated to paste at the temperature of 55 ℃ under the vacuum degree of 0.09Mpa and then dried to constant weight.
7. A method of processing tea seed cake according to claim 6, wherein: in the step S7, the calculation formulas of the purity and the yield of the tea saponin are as follows:
tea saponin purity = (a-0.0626) ×v×n/8.0918×m 1 *100％；
Tea saponin yield = tea saponin purity M 2 /M 3 *100％；
Wherein:
a is absorbance; v is the volume ml of the solution; n is the multiple of the dilution of the solution; m is M 1 is Measuring the amount mg of the tea saponin weighed by the A; m is M 2 The amount of tea saponin is mg; m is M 3 Is the weight of the defatted tea seed cake.
8. A method of processing tea seed cake according to claim 7, wherein: in the step S4, at least one of ultrasonic leaching and water bath leaching is used, and the tea saponin can also be extracted by matching ultrasonic leaching with water bath leaching.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103570794A (en) * | 2013-11-06 | 2014-02-12 | 东北农业大学 | Extracting method of camellia seed saponin |
| CN112409438A (en) * | 2020-12-18 | 2021-02-26 | 南京泽朗医药技术有限公司 | Process for extracting tea saponin by ultrasonic water bath |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103570794A (en) * | 2013-11-06 | 2014-02-12 | 东北农业大学 | Extracting method of camellia seed saponin |
| CN112409438A (en) * | 2020-12-18 | 2021-02-26 | 南京泽朗医药技术有限公司 | Process for extracting tea saponin by ultrasonic water bath |
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| 曹江绒: "茶皂素的提取、纯化及在洗发液中的应用研究", 《硕士学位论文》, pages 16 * |
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