CN113061155A - Method for extracting tea saponin from camellia seeds - Google Patents
Method for extracting tea saponin from camellia seeds Download PDFInfo
- Publication number
- CN113061155A CN113061155A CN202110288864.8A CN202110288864A CN113061155A CN 113061155 A CN113061155 A CN 113061155A CN 202110288864 A CN202110288864 A CN 202110288864A CN 113061155 A CN113061155 A CN 113061155A
- Authority
- CN
- China
- Prior art keywords
- extraction
- tea saponin
- seeds
- powder
- transferring
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
- Genetics & Genomics (AREA)
- Molecular Biology (AREA)
- Steroid Compounds (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a method for extracting tea saponin from camellia seeds, belonging to the technical field of plant extraction processes. It comprises the following steps: (1) selecting oil tea seeds, stripping shells, taking out the seeds, cleaning and drying; (2) transferring the seeds into an electric heating blast drier, removing moisture, and then putting the seeds into a crusher for crushing to obtain seed powder; (3) transferring the grain powder into a Soxhlet extractor for extraction, and then naturally drying to obtain extracted powder; (4) transferring the powder into a water bath for extraction, then naturally drying, and recovering the extracted powder; (5) transferring the powder into an extraction tank for extraction, and recovering an extraction liquid; (6) concentrating the extract under reduced pressure to obtain viscous substance; (7) transferring the viscous substance into a low-temperature spray dryer. Tests show that the parameters of the tea saponin, such as yield, extraction purity, DPPH free radical clearance and the like, have better significant differences.
Description
Technical Field
The invention belongs to the technical field of plant extraction processes, and particularly relates to a method for extracting tea saponin from camellia seeds.
Background
China has rich camellia oleifera resources, is the country with the highest yield, the widest distribution and the most varieties of camellia oleifera seeds in the world, is mainly distributed in Yangtze river basin, produces more than 60 ten thousand tons of camellia oleifera seeds annually, and has the annual average yield of camellia oleifera seed byproducts, namely camellia dregs, of about 40 ten thousand tons. Tea saponin is oleanane type pentacyclic triterpene saponin, and is a mixture with complex structure formed by sapogenin (namely aglycone), saccharide and organic acid. The non-ionic natural surfactant has wide application, is a non-ionic natural surfactant with excellent performance, has strong foaming, emulsifying, dispersing and other effects, has the physiological activities of anti-permeability, anti-inflammation, analgesia, anticancer and the like, and can be widely applied to the industries of daily chemicals, medicines, foods, building materials, pesticides and the like. At present, the method for extracting tea saponin at home and abroad mainly comprises a water immersion method, an organic solvent method and a new method popularized and developed on the basis of the water immersion method and the organic solvent method. The water leaching method has the defects of low yield and purity of the tea saponin and limitation of the application range of the tea saponin. The organic solvent method usually uses aqueous methanol or aqueous ethanol as an extractant, and most of the methods use ethanol for extraction due to high cost and toxicity of methanol. The method has the advantages of short time consumption, and relatively high yield and purity. However, the traditional extraction process of tea saponin is easy to cause inactivation of tea saponin, such as its antioxidant property.
For example, the chinese invention patent, application No.: CN201910463338.3, publication No.: CN 110092810B discloses a method for extracting and refining tea saponin, which comprises the following steps:
' a method for extracting and refining tea saponin, which comprises the following steps:
(1) pretreatment of raw materials: drying the raw materials, crushing and sieving to obtain raw material powder;
(2) adding an organic solvent into the raw material powder obtained in the step (1), and uniformly stirring to obtain a feed liquid;
(3) adjusting the temperature of the feed liquid in the step (2), and performing heat preservation pretreatment;
(4) carrying out solid-liquid separation on the feed liquid obtained in the step (3) under the condition of heat preservation;
(5) carrying out nanofiltration separation on the liquid obtained in the step (4), and adding a solvent into trapped liquid for dilution;
(6) combining the trapped liquids obtained in the step (5), and drying in vacuum to obtain high-purity tea saponin;
the raw material in the step (1) is camellia seed meal.
And (2) sieving by a 60-mesh sieve in the step (1).
And (2) drying in the step (1) is natural drying.
The weight ratio of the raw material powder to the organic solvent in the step (2) is 1: 10.
The organic solvent in the step (2) is a mixed solvent of a polar organic solvent and a non-polar organic solvent.
The mixed solvent of the polar organic solvent and the non-polar organic solvent is as follows: the ratio of n-butanol to ethanol was 10: 1 (volume ratio).
The heat preservation pretreatment in the step (3) is carried out at the temperature of 80 ℃; the heat preservation pretreatment time is 4 h.
And (4) keeping the temperature of the heat preservation condition in the step (4) the same as the temperature in the heat preservation pretreatment step in the step (3).
And (4) carrying out solid-liquid separation by filtering or centrifuging, wherein the washing times are 3 times.
And (4) drying the solid obtained in the step (4), and directly using the dried solid as feed or other purposes, wherein whether the organic solvent is recovered or not can be determined according to requirements.
And (5) diluting, wherein the added solvent is ethanol, and the addition amount is 2 times of the volume of the trapped fluid.
In the step (5), the number of times of adding the solvent to the retentate to dilute is 3.
The interception molecular weight of the nanofiltration membrane used in the nanofiltration operation in the step (5) is 900-.
However, the above patent utilizes camellia seed meal, wherein the camellia seed meal is a byproduct of camellia seed after squeezing, the content of tea saponin is low, and the tea saponin is oxidized and damaged more, although a certain amount of tea saponin is extracted, the antioxidant activity of the tea saponin is low, and the removal of DPPH free radicals cannot be effectively realized.
Disclosure of Invention
1. Problems to be solved
Aiming at the problems in the prior art, the invention provides the method for extracting the tea saponin from the camellia seeds, and the parameters such as the yield, the extraction purity, the removal rate of DPPH free radicals and the like of the tea saponin have better significant difference.
2. Technical scheme
In order to solve the above problems, the present invention adopts the following technical solutions.
A method for extracting tea saponin from oil tea seeds comprises the following steps:
(1) selecting oil tea seeds, stripping shells, taking out the seeds, cleaning and drying;
(2) transferring the seeds treated in the step (1) into an electric heating forced air dryer to remove moisture, and then placing the seeds into a crusher to be crushed to obtain seed powder;
(3) transferring the seed powder treated in the step (2) to a Soxhlet extractor for extraction, and then naturally drying in the air to obtain extracted powder;
(4) transferring the powder treated in the step (3) to a water bath for extraction, then naturally drying, and recovering the extracted powder;
(5) transferring the powder treated in the step (4) to an extraction tank for extraction, and recovering an extraction liquid;
(6) carrying out reduced pressure concentration on the extract liquid treated in the step (5) to obtain a viscous substance;
(7) and (4) transferring the viscous substance treated in the step (6) to a low-temperature spray dryer.
In the method for extracting tea saponin from camellia seeds, the seeds in the step (1) need to be subjected to epidermis removal;
and (2) cleaning the grains in the step (1) by using a cleaning agent, wherein the cleaning agent used for cleaning is a PBS (phosphate buffer solution) containing EDTA, and the mass concentration of the EDTA is 0.1 mM.
In the method for extracting tea saponin from camellia seeds, the average water content of the seeds subjected to water removal in the step (2) is less than 3%;
the grain size of the grain powder in the step (2) is 200 meshes.
In the method for extracting tea saponin from camellia seeds, the extracting agent used in the step (3) is a mixture of petroleum ether, butyl acetate and isopropanol, wherein the dosage ratio of the petroleum ether, the butyl acetate and the isopropanol is 1: 5: 2.
in the method for extracting tea saponin from camellia seeds, the water bath time in the step (4) is 2 hours;
extracting agents of the water bath in the step (4) are an ethanol solution with the mass concentration of 85% and a dimethyl carbonate solution with the mass concentration of 20%, wherein the dosage ratio of the ethanol solution to the dimethyl carbonate solution is 1: 2.
in the method for extracting tea saponin from camellia seeds, after the extraction tank is vacuumized in the step (5), 10-40 times of deionized water in powder mass is put into the extraction tank, and subcritical extraction is carried out under the conditions that the extraction temperature is 160 ℃, the extraction pressure is 5MPa, the extraction time is 30min and the extraction times are 3 times.
In the method for extracting tea saponin from camellia seeds, an extraction aid is further added, and the dosage ratio of the extraction aid to the powder is 8: 1;
the extraction auxiliary agent comprises acetonitrile, tartaric acid and carbon tetrachloride, wherein the dosage ratio of the acetonitrile to the tartaric acid to the carbon tetrachloride is 2: 1: 5.
in the method for extracting tea saponin from camellia seeds, the temperature for reduced pressure concentration in the step (6) is set to be 4 ℃;
the volume ratio of the vacuum concentration in the step (6) is 6.
In the method for extracting tea saponin from camellia seeds, the temperature of the low-temperature spray drying in the step (7) is 30 ℃.
In the method for extracting tea saponin from camellia seeds, the average particle size of the powder after low-temperature spray drying in the step (7) is 200 μm.
3. Advantageous effects
Compared with the prior art, the invention has the beneficial effects that:
the extraction method of the invention has better significant differences in the parameters of the yield, the extraction purity, the removal rate of DPPH free radicals and the like of the tea saponin. In the prior art, the key parameters of the Soxhlet extraction method are set, and when the dosage ratio of petroleum ether, butyl acetate and isopropanol is 1: 5: 2, the yield and the extraction purity of the tea saponin can be effectively optimized, and simultaneously, an extraction auxiliary agent is innovatively introduced into the subcritical extraction process, wherein the extraction auxiliary agent is a mixture of acetonitrile, tartaric acid and carbon tetrachloride, and the mass ratio of the acetonitrile to the tartaric acid to the carbon tetrachloride is 2: 1: 5, the yield and the extraction purity of the tea saponin are greatly improved; in addition, compared with a plurality of prior arts, the yield of the tea saponin is 24.5%, the extraction purity of the tea saponin is 95.7%, and the DPP H free radical clearance rate is as high as 92.7%.
Detailed Description
The invention is further described with reference to specific examples.
Example 1
The method for extracting tea saponin from camellia seeds comprises the following steps:
(1) selecting oil tea seeds, stripping shells, taking out the seeds, cleaning and drying; the seed needs to be subjected to epidermis removal;
cleaning the grains in the step (1) by using a cleaning agent, wherein the cleaning agent used for cleaning is a PBS (phosphate buffer solution) containing EDTA (ethylene diamine tetraacetic acid), and the mass concentration of the EDTA is 0.1 mM; in general, the seeds are cleaned by clear water, but impurities on the surfaces of the seeds cannot be easily removed by the clear water treatment, and the tea saponin is easily damaged by the clear water;
(2) transferring the seeds treated in the step (1) into an electric heating forced air dryer to remove moisture, and then placing the seeds into a crusher to be crushed to obtain seed powder; wherein the average water content of the kernels after water removal is less than 3%; wherein the grain powder has a particle size of 200 meshes; the water content in the seeds is reduced, and the degradation of tea saponin by enzyme in the seeds can be inhibited;
(3) transferring the seed powder treated in the step (2) to a Soxhlet extractor for extraction, and then naturally drying in the air to obtain extracted powder; the extracting agent used for extraction is a mixture of petroleum ether, butyl acetate and isopropanol, wherein the dosage ratio of the petroleum ether to the butyl acetate to the isopropanol is 1: 5: 2; in the laboratory, soxhlet extraction was the key step, and the following tests were performed:
TABLE 1 test results
As can be seen from table 1, the three substances have important influence on the yield and extraction purity of tea saponin, and the yield and extraction purity of tea saponin are lower by changing the dosage ratio of the three substances or adopting two combinations of the three substances, which indicates that the three substances have synergistic effect;
(4) transferring the powder treated in the step (3) into a water bath pot for extraction, wherein the water bath time is 2 hours, then naturally drying, and recovering the extracted powder; the water bath extracting agents are an ethanol solution with the mass concentration of 85% and a dimethyl carbonate solution with the mass concentration of 20%, wherein the dosage ratio of the ethanol solution to the dimethyl carbonate solution is 1: 2; it should be noted that, in general, an ethanol solution is generally used for water bath extraction, and in the searching process, it is found that the yield and the extraction purity of tea saponin cannot be effectively improved (the average reduction is about 5.2%) only by using the ethanol solution, and dimethyl carbonate of a common water treatment agent is added, and it is found that the dimethyl carbonate can be mutually dissolved with the ethanol solution, but the effect of using the dimethyl carbonate alone is reduced by 8.6%, if the mass concentration of the dimethyl carbonate solution is changed to 10% or the dosage ratio of the dimethyl carbonate solution to the ethanol solution is changed to 1:1, the overall effect is reduced by about 3.5 percent on average, if the mass concentration of the dimethyl carbonate solution is changed to 30 percent or the dosage ratio of the dimethyl carbonate solution to the dimethyl carbonate solution is changed to 2: 1, the overall effect is reduced by about 3.1 percent on average;
(5) transferring the powder treated in the step (4) to an extraction tank for extraction, and recovering an extraction liquid; after the extraction tank is vacuumized, putting deionized water with the mass 30 times that of the powder into the extraction tank, and performing subcritical extraction under the conditions that the extraction temperature is 160 ℃, the extraction pressure is 5MPa, the extraction time is 30min and the extraction times are 3 times; and adding an extraction aid, wherein the dosage ratio of the extraction aid to the powder is 8: 1; the extraction auxiliary agent comprises acetonitrile, tartaric acid and carbon tetrachloride, wherein the dosage ratio of the acetonitrile to the tartaric acid to the carbon tetrachloride is 2: 1: 5; in the subcritical extraction process, a suitable extraction auxiliary agent plays a key role, acetonitrile, tartaric acid and carbon tetrachloride are rarely applied to the extraction of the tea saponin, and particularly, substances of the acetonitrile, the tartaric acid and the carbon tetrachloride are mixed for use, as shown in table 2, the acetonitrile, the tartaric acid and the carbon tetrachloride have synergistic interaction, so that the yield and the extraction purity of the tea saponin are improved.
TABLE 2 test results
(6) Carrying out reduced pressure concentration on the extract liquid treated in the step (5) to obtain a viscous substance; wherein the temperature of the reduced pressure concentration is set to 4 ℃; wherein the volume ratio of the decompression concentration is 6;
(7) transferring the viscous substance treated in the step (6) to a low-temperature spray dryer; wherein the low-temperature spray drying temperature is 30 ℃; wherein the average particle diameter of the powder after low-temperature spray drying is 200 μm.
Comparative example 1
Chinese invention patent, application number: CN201910581927.1, publication No.: CN112225774A discloses a novel method for extracting tea saponin with high purity and high yield, which comprises the following steps:
500g of camellia seed meal is dried and crushed, and then is mixed with 50g of grinding aid for solid grinding;
(2) adding 1000ml of water into the mixture obtained in the step (1), stirring, extracting and filtering to obtain filtrate; stirring at 120 deg.C for 1.5 h;
(3) adding 100ml of organic acid into the filtrate obtained in the step (2) to obtain a crystalline tea saponin crude product;
(4) heating the crystal at 160 deg.C for 1.5h, adding 25ml of aqueous ethanol-acetone composite solvent, and stirring for 2 h;
(5) adding 28g of sterol complexing agent into the obtained mixture for complexing treatment; vacuum concentrating at low temperature for 3 hr, and vacuum filtering and drying to obtain tea saponin complex;
(6) carrying out decomplexing separation treatment on the mixture obtained in the step (5), and carrying out hot filtration to obtain high-purity tea saponin;
(7) separating and recovering the solvent, filtering or centrifugally separating the leaching solution, and simultaneously decompressing and evaporating to recover the organic solvent in the leaching solution to obtain a tea saponin aqueous solution; then removing water for 1h to obtain a tea saponin mixture;
(8) and (5) decolorizing and spray drying the tea saponin solution in the step (7) to obtain high-purity tea saponin.
Comparative example 2
Chinese invention patent, application number: CN202011072610.4, publication No.: CN112194700A discloses a preparation method of natural high-purity tea saponin with high-efficiency decontamination, which comprises the following specific technical scheme:
' a preparation system of natural high-purity tea saponin with high-efficient decontamination, the method comprises the following steps:
step one, placing the tea seed cake in a tea saponin preparation system for milling;
step two, putting the powder into water to be mixed to obtain a mixed solution;
step three, centrifuging the mixed solution to extract supernatant;
step four, preparing the tea saponin by using the supernatant as a raw material;
the preparation method of the natural high-purity tea saponin with high decontamination efficiency also comprises a preparation system of the tea saponin; tea saponin's preparation system includes mounting bracket I2, mount pad 201, mounting bracket II 202, system platform 3 just, axle 301, motor I302, hydraulic push rod 4 and pressure head 401, two mount pads 201 of left side rigid coupling of mounting bracket I2 upper end, the lower extreme rigid coupling axle 301 of system platform 3 just, the both ends of axle 301 are rotated respectively and are connected on two mount pads 201, the output shaft and the axle 301 rigid coupling of motor I302, I302 rigid coupling of motor is on mount pad 201, II 202 rigid couplings of mounting bracket are in the upper end of mounting bracket I2, hydraulic push rod 4 installs on mounting bracket I2, the expansion end rigid coupling pressure head 401 of hydraulic push rod 4, pressure head 401 is located system platform 3 just over. Place the tea-seed cake on primary system platform 3, start hydraulic rod 4, utilize hydraulic rod 4 to drive pressure head 401 and crush the tea-seed cake. The starter motor I302, the output shaft of motor I302 drives and just makes 3 rotations on the platform, emptys the dried tea seed cake after will crushing, and the dried tea seed cake after the crushing does benefit to the solid extraction of liquid ".
Comparative example 3
Chinese invention patent, application number: CN202011156367.4, publication No.: CN112110979A discloses a method for extracting tea saponin, the specific technical scheme is as follows:
drying tea seed cake at a constant temperature of 60 ℃ to constant weight, crushing and sieving with a 50-mesh sieve to obtain tea seed cake powder with the particle size of less than 0.27 mm, degreasing the tea seed cake powder by a Soxhlet extraction method, and drying at the constant temperature of 60 ℃ to constant weight to obtain a tea seed cake raw material;
(2) mixing 100g of the tea seed cake raw material obtained in the step (1) with 2L of ethanol-water solution (the ethanol content is 60 vol%), performing ultrasonic-assisted extraction for 3 hours at 70 ℃ in a water bath, filtering and collecting filtrate by using filter paper, repeatedly extracting for 2 times, combining the filtrate extracted for 3 times to obtain an extracting solution, performing rotary evaporation on the extracting solution to obtain an extract paste, and performing freeze drying to obtain a crude product of tea saponin;
(3) mixing 20g of the crude tea saponin product obtained in the step (2) with 200g of water to obtain a tea saponin solution, separating the tea saponin solution by an AB-8 macroporous adsorption resin column (the resin amount in the resin column is 30 mL) at the flow rate of 2BV/h, washing the resin column with 135mL of distilled water, eluting with 150mL of ethanol-water solution (the ethanol content is 70 vol%) at the flow rate of 2BV/h, and collecting eluent;
(4) and (3) performing rotary evaporation on the eluent obtained in the step (3) to remove ethanol, diluting the eluent with distilled water until the content of tea saponin is 1 mass%, adding a flocculant solution (the content of chitosan in the flocculant solution is 0.1 mass%, sodium carboxymethylcellulose is 0.067 mass% and chitin is 0.033 mass%) according to 3% of the volume of the tea saponin aqueous solution, stirring for 5min, standing for 1.5h at room temperature, centrifuging at 3000r/min, collecting clear liquor, and performing freeze drying on the clear liquor to obtain the tea saponin.
Comparative example 4
Chinese invention patent, application number: CN202010668797.8, publication No.: CN112047994A discloses a method for extracting tea saponin from camellia seed meal, the specific technical scheme is as follows:
the method specifically comprises the following steps:
step S1: pretreatment of camellia seed meal: pulverizing Camellia seed meal until the particle size of the Camellia seed meal is 60 meshes, drying, adding oil extraction agent, i.e. petroleum ether, and separating to obtain tea oil and defatted tea cake.
Step S2: and (3) extraction and concentration: and (4) adding normal propyl alcohol into the degreased tea cake obtained in the step (S1), carrying out ultrasonic treatment, and then concentrating and separating to obtain primary filtrate and primary filter residue. In this step, the temperature of the ultrasonic treatment was 60 ℃, the ultrasonic power was 600W, and the concentration of n-propanol added was 80% and the pH was 11. The amount of n-propanol added is 1:12 by volume solid-liquid ratio, and the extraction time is 3 hours.
Step S3: precipitation and impurity removal: adding a precipitator, namely acetone, into the primary filtrate obtained in the step S2, and then performing centrifugal separation to obtain a secondary filtrate and a secondary filter residue, wherein the secondary filter residue is a crude product of the tea saponin;
step S4: washing and drying: and (4) washing and separating the solid obtained by separating in the step S3, wherein the washing agent is acetone.
Step S5: and drying to obtain a separated and purified tea saponin product'.
Comparative example 5
Chinese invention patent, application number: CN201910615565.3, publication No.: CN110437299B discloses a method for extracting tea saponin, which comprises the following steps:
the invention provides a method for extracting tea saponin, which comprises the following steps:
s1, crushing the tea seed cake, sieving, adding petroleum ether into the crushed tea seed cake, wherein the material-liquid ratio is 1: 4, stirring for 25min, and performing centrifugal separation to obtain defatted tea seed cake;
s2, introducing water vapor into the degreased tea seed cake to keep the internal gas humidity at 24%, sealing and keeping for 30min, taking out the wet tea seed cake, freezing for 24h at-16 ℃, then unfreezing at normal temperature, and repeating the freezing-unfreezing operation for 2 times to obtain the pretreated tea seed cake;
s3, placing the pre-treated tea seed meal into a percolation cylinder, adding 75% ethanol solution for soaking for 30min, then adopting 75% ethanol solution for percolation treatment, wherein the total amount of the ethanol solution for percolation is 4.5 times of the initial weight of the tea seed meal, the percolation speed is 4mL of percolate flowing out every 1000g of the initial tea seed meal per minute, and collecting the percolate;
s4, recovering ethanol from the percolate under reduced pressure, adding 9 times of water, adjusting the pH to 10.0, stirring, standing for 5-8 h, and filtering to obtain a refined extract;
s5, dropwise adding a hydrochloric acid solution into the refined extract until the pH value is 2.5, stirring, standing, filtering, washing, dissolving with a 95% ethanol solution, dropwise adding acetone, standing, filtering and drying to obtain the product.
Example 2
The tea saponin prepared in example 1 and the tea saponin prepared in comparative examples 1 to 5 were selected and analyzed for the yield and extraction purity of tea saponin (see the following documents: Yunhui, Chenhaiguang, Wubo, et al. n-propanol extraction process [ J ] food science, 2013,034(002):58-62.) and the actual antioxidant activity of the extracted tea saponin (see the following documents: Jiaojiao, extraction and purification of tea saponin in water phase after extracting camellia seed oil by aqueous medium method and property research [ D ]). As shown in table 3, the extraction method of the present application has high extraction purity and yield of tea saponin, high clearance rate of D PPH free radicals, and other indexes, and embodies significant differences.
TABLE 3 alignment assay
While the invention has been described in further detail in connection with specific embodiments thereof, it will be understood that the invention is not limited thereto, and that various other modifications and substitutions may be made by those skilled in the art without departing from the spirit of the invention, which should be considered to be within the scope of the invention as defined by the appended claims.
Claims (10)
1. A method for extracting tea saponin from oil tea seeds comprises the following steps:
(1) selecting oil tea seeds, stripping shells, taking out the seeds, cleaning and drying;
(2) transferring the seeds treated in the step (1) into an electric heating forced air dryer to remove moisture, and then placing the seeds into a crusher to be crushed to obtain seed powder;
(3) transferring the seed powder treated in the step (2) to a Soxhlet extractor for extraction, and then naturally drying in the air to obtain extracted powder;
(4) transferring the powder treated in the step (3) to a water bath for extraction, then naturally drying, and recovering the extracted powder;
(5) transferring the powder treated in the step (4) to an extraction tank for extraction, and recovering an extraction liquid;
(6) carrying out reduced pressure concentration on the extract liquid treated in the step (5) to obtain a viscous substance;
(7) and (4) transferring the viscous substance treated in the step (6) to a low-temperature spray dryer.
2. The method for extracting tea saponin from camellia seeds as claimed in claim 1, wherein:
in the step (1), the seed needs to be subjected to epidermis removal;
and (2) cleaning the grains in the step (1) by using a cleaning agent, wherein the cleaning agent used for cleaning is a PBS (phosphate buffer solution) containing EDTA, and the mass concentration of the EDTA is 0.1 mM.
3. The method for extracting tea saponin from camellia seeds as claimed in claim 1, wherein:
the average water content of the kernels subjected to water removal in the step (2) is less than 3 percent;
the grain size of the grain powder in the step (2) is 200 meshes.
4. The method for extracting tea saponin from camellia seeds as claimed in claim 1, wherein:
the extracting agent used in the extraction in the step (3) is a mixture of petroleum ether, butyl acetate and isopropanol, wherein the dosage ratio of the petroleum ether to the butyl acetate to the isopropanol is 1: 5: 2.
5. the method for extracting tea saponin from camellia seeds as claimed in claim 1, wherein:
the water bath time in the step (4) is 2 hours;
extracting agents of the water bath in the step (4) are an ethanol solution with the mass concentration of 85% and a dimethyl carbonate solution with the mass concentration of 20%, wherein the dosage ratio of the ethanol solution to the dimethyl carbonate solution is 1: 2.
6. the method for extracting tea saponin from camellia seeds as claimed in claim 1, wherein:
and (5) after the extraction tank is vacuumized, putting 10-40 times of deionized water in the extraction tank, and performing subcritical extraction under the conditions that the extraction temperature is 160 ℃, the extraction pressure is 5MPa, the extraction time is 30min and the extraction times are 3 times.
7. The method for extracting tea saponin from camellia seeds as claimed in claim 6, wherein:
and adding an extraction aid, wherein the dosage ratio of the extraction aid to the powder is 8: 1;
the extraction auxiliary agent comprises acetonitrile, tartaric acid and carbon tetrachloride, wherein the dosage ratio of the acetonitrile to the tartaric acid to the carbon tetrachloride is 2: 1: 5.
8. the method for extracting tea saponin from camellia seeds as claimed in claim 1, wherein:
the temperature of the reduced pressure concentration in the step (6) is set to be 4 ℃;
the volume ratio of the vacuum concentration in the step (6) is 6.
9. The method for extracting tea saponin from camellia seeds as claimed in claim 1, wherein:
the temperature of the low-temperature spray drying in the step (7) is 30 ℃.
10. The method for extracting tea saponin from camellia seeds as claimed in claim 9, wherein:
the average particle size of the powder after low-temperature spray drying in the step (7) is 200 μm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110288864.8A CN113061155A (en) | 2021-03-18 | 2021-03-18 | Method for extracting tea saponin from camellia seeds |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110288864.8A CN113061155A (en) | 2021-03-18 | 2021-03-18 | Method for extracting tea saponin from camellia seeds |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113061155A true CN113061155A (en) | 2021-07-02 |
Family
ID=76561224
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110288864.8A Pending CN113061155A (en) | 2021-03-18 | 2021-03-18 | Method for extracting tea saponin from camellia seeds |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113061155A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115138096A (en) * | 2022-07-07 | 2022-10-04 | 广州美林生态科技有限公司 | Method for extracting tea saponin by subcritical ethanol and/or methanol |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107056876B (en) * | 2017-05-22 | 2019-05-24 | 江西乔盛茶皂素科技有限公司 | A method of extracting high-purity tea saponin from camellia seed meal |
| CN110437299B (en) * | 2019-07-09 | 2020-09-18 | 合肥学院 | Extraction method of tea saponin |
| CN112047994A (en) * | 2020-07-13 | 2020-12-08 | 安徽裕民生态农业有限公司 | Method for extracting tea saponin from camellia seed meal |
| CN112110979A (en) * | 2020-10-26 | 2020-12-22 | 长沙中战茶油集团有限公司 | Method for extracting tea saponin |
| CN112194700A (en) * | 2020-10-09 | 2021-01-08 | 张利民 | Preparation method of natural high-purity tea saponin with high decontamination efficiency |
| CN112225774A (en) * | 2019-06-30 | 2021-01-15 | 刘海秀 | Novel method for extracting tea saponin with high purity and high extraction rate |
-
2021
- 2021-03-18 CN CN202110288864.8A patent/CN113061155A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107056876B (en) * | 2017-05-22 | 2019-05-24 | 江西乔盛茶皂素科技有限公司 | A method of extracting high-purity tea saponin from camellia seed meal |
| CN112225774A (en) * | 2019-06-30 | 2021-01-15 | 刘海秀 | Novel method for extracting tea saponin with high purity and high extraction rate |
| CN110437299B (en) * | 2019-07-09 | 2020-09-18 | 合肥学院 | Extraction method of tea saponin |
| CN112047994A (en) * | 2020-07-13 | 2020-12-08 | 安徽裕民生态农业有限公司 | Method for extracting tea saponin from camellia seed meal |
| CN112194700A (en) * | 2020-10-09 | 2021-01-08 | 张利民 | Preparation method of natural high-purity tea saponin with high decontamination efficiency |
| CN112110979A (en) * | 2020-10-26 | 2020-12-22 | 长沙中战茶油集团有限公司 | Method for extracting tea saponin |
Non-Patent Citations (3)
| Title |
|---|
| 于辉等: "正丙醇提取茶皂素工艺", 《食品科学》 * |
| 朱新亮等: "亚临界萃取技术在食用油及农产品加工中的应用", 《粮油与饲料科技》 * |
| 顾姣: "《2017年江南大学硕士论文》", 30 June 2017 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115138096A (en) * | 2022-07-07 | 2022-10-04 | 广州美林生态科技有限公司 | Method for extracting tea saponin by subcritical ethanol and/or methanol |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US12109509B2 (en) | Ultrasonic composite acidic water extraction method for cordyceps polysaccharide and cordycepin in Cordyceps militaris | |
| CN108752231B (en) | Method for extracting theanine from sweet tea and simultaneously extracting rubusoside and tea polyphenol | |
| CN109674843B (en) | Extraction and purification method for comprehensively utilizing dried momordica grosvenori | |
| CN110272932B (en) | Preparation method of ganoderma lucidum spore powder polysaccharide peptide | |
| CN112110979B (en) | Method for extracting tea saponin | |
| CN101531690A (en) | New technology for extracting tea saponin and tea seed oil from tea seeds by using water as solvent | |
| CN110684128B (en) | Method for extracting and refining polygonatum sibiricum polysaccharide | |
| CN101935278A (en) | Method for extracting, separating and purifying chlorogenic acid through folium cortex eucommiae | |
| CN111603500B (en) | Semen cassiae extract and process technology for comprehensively developing and utilizing semen cassiae | |
| CN103012544B (en) | A kind of method extracting saponin and polysaccharide from tea seed grouts | |
| CN102060728A (en) | Method for extracting capsorubin and capsaicin from chillies | |
| CN104177370A (en) | Method for preparing high-content sesamin from sesame seed meal | |
| CN1754883A (en) | Production process for extracting tea saponin from tea-oil tree cake by using water as dissoluent | |
| CN113913029B (en) | Method for preparing effective components of gardenia jasminoides ellis | |
| CN111072618A (en) | Method for conveniently and rapidly purifying dihydromyricetin from Ampelopsis grossedentata leaves | |
| CN112225774A (en) | Novel method for extracting tea saponin with high purity and high extraction rate | |
| CN113061155A (en) | Method for extracting tea saponin from camellia seeds | |
| JP6703562B2 (en) | Method for producing polyphenol composition from bagasse | |
| EP3505525B1 (en) | Method for preparing rubusoside | |
| CN113897406A (en) | Method for extracting and purifying salidroside from rhodiola rosea powder | |
| CN107190028B (en) | The extracting method of ferulic acid in a kind of rice bran meal | |
| CN110917240B (en) | Continuous method for separating multiple effective components from cyclocarya paliurus | |
| CN108997359B (en) | Method for extracting chlorophyll from stevioside production waste residues | |
| CN104788515B (en) | Method for preparing high-purity water-soluble oleuropein by reduced pressure ultrasonic-assisted extraction | |
| CN113773360B (en) | Method for separating mogrol from fructus momordicae |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210702 |
|
| RJ01 | Rejection of invention patent application after publication |