CN114621830B - Oil tea cake extract, preparation method and application thereof - Google Patents
Oil tea cake extract, preparation method and application thereof Download PDFInfo
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- CN114621830B CN114621830B CN202210055488.2A CN202210055488A CN114621830B CN 114621830 B CN114621830 B CN 114621830B CN 202210055488 A CN202210055488 A CN 202210055488A CN 114621830 B CN114621830 B CN 114621830B
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- 241001122767 Theaceae Species 0.000 title claims abstract description 100
- 239000000284 extract Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000000693 micelle Substances 0.000 claims abstract description 31
- 238000000605 extraction Methods 0.000 claims abstract description 30
- 239000001397 quillaja saponaria molina bark Substances 0.000 claims abstract description 25
- 229930182490 saponin Natural products 0.000 claims abstract description 25
- 150000007949 saponins Chemical class 0.000 claims abstract description 25
- 239000004094 surface-active agent Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000003960 organic solvent Substances 0.000 claims abstract description 9
- 239000007864 aqueous solution Substances 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 35
- 239000000843 powder Substances 0.000 claims description 24
- 238000000926 separation method Methods 0.000 claims description 18
- 239000006228 supernatant Substances 0.000 claims description 18
- 239000007853 buffer solution Substances 0.000 claims description 13
- 239000012074 organic phase Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000000047 product Substances 0.000 claims description 10
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 238000007873 sieving Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 7
- NHTMVDHEPJAVLT-UHFFFAOYSA-N Isooctane Chemical compound CC(C)CC(C)(C)C NHTMVDHEPJAVLT-UHFFFAOYSA-N 0.000 claims description 6
- 238000004440 column chromatography Methods 0.000 claims description 6
- JVSWJIKNEAIKJW-UHFFFAOYSA-N dimethyl-hexane Natural products CCCCCC(C)C JVSWJIKNEAIKJW-UHFFFAOYSA-N 0.000 claims description 6
- 238000004090 dissolution Methods 0.000 claims description 6
- 235000012054 meals Nutrition 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000012071 phase Substances 0.000 claims description 6
- 238000002137 ultrasound extraction Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 4
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 4
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 4
- XKBGEWXEAPTVCK-UHFFFAOYSA-M methyltrioctylammonium chloride Chemical compound [Cl-].CCCCCCCC[N+](C)(CCCCCCCC)CCCCCCCC XKBGEWXEAPTVCK-UHFFFAOYSA-M 0.000 claims description 4
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 4
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical class [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 3
- 239000003599 detergent Substances 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 claims description 3
- 235000010234 sodium benzoate Nutrition 0.000 claims description 3
- 239000004299 sodium benzoate Substances 0.000 claims description 3
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 2
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 claims description 2
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 claims description 2
- QZXSMBBFBXPQHI-UHFFFAOYSA-N N-(dodecanoyl)ethanolamine Chemical compound CCCCCCCCCCCC(=O)NCCO QZXSMBBFBXPQHI-UHFFFAOYSA-N 0.000 claims description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 2
- HDMXIELEUKTYFR-UHFFFAOYSA-N bis(2-ethylhexyl) butanedioate;sodium Chemical compound [Na].CCCCC(CC)COC(=O)CCC(=O)OCC(CC)CCCC HDMXIELEUKTYFR-UHFFFAOYSA-N 0.000 claims description 2
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 claims description 2
- 150000002191 fatty alcohols Chemical class 0.000 claims description 2
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 2
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 2
- 235000011152 sodium sulphate Nutrition 0.000 claims description 2
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 abstract description 3
- 239000003921 oil Substances 0.000 description 55
- 239000010779 crude oil Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 5
- 102000004169 proteins and genes Human genes 0.000 description 5
- 108090000623 proteins and genes Proteins 0.000 description 5
- 241000209507 Camellia Species 0.000 description 3
- 235000018597 common camellia Nutrition 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 238000005202 decontamination Methods 0.000 description 2
- 230000003588 decontaminative effect Effects 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
- 238000005187 foaming Methods 0.000 description 2
- 239000004519 grease Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 230000001139 anti-pruritic effect Effects 0.000 description 1
- 239000003908 antipruritic agent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 230000009881 electrostatic interaction Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/86—Mixtures of anionic, cationic, and non-ionic compounds
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
- C11D3/046—Salts
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/20—Organic compounds containing oxygen
- C11D3/2075—Carboxylic acids-salts thereof
- C11D3/2079—Monocarboxylic acids-salts thereof
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/20—Organic compounds containing oxygen
- C11D3/2075—Carboxylic acids-salts thereof
- C11D3/2082—Polycarboxylic acids-salts thereof
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/26—Organic compounds containing nitrogen
- C11D3/33—Amino carboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
- C11D1/22—Sulfonic acids or sulfuric acid esters; Salts thereof derived from aromatic compounds
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
- C11D1/28—Sulfonation products derived from fatty acids or their derivatives, e.g. esters, amides
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
- C11D1/29—Sulfates of polyoxyalkylene ethers
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/38—Cationic compounds
- C11D1/62—Quaternary ammonium compounds
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/66—Non-ionic compounds
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/66—Non-ionic compounds
- C11D1/662—Carbohydrates or derivatives
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- Chemical & Material Sciences (AREA)
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- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Emergency Medicine (AREA)
- Inorganic Chemistry (AREA)
- Extraction Or Liquid Replacement (AREA)
- Tea And Coffee (AREA)
Abstract
The invention provides a preparation method of an oil tea cake extract, which is characterized in that a reverse micelle system formed by an aqueous solution containing a surfactant and a nonpolar organic solvent is combined with an ultrasonic method to extract tea saponin in the oil tea cake, and the content of the tea saponin in the obtained oil tea cake extract is greatly improved through front extraction, centrifugation and back extraction, so that the process flow is shortened.
Description
Technical Field
The invention belongs to the technical field of plant extraction, and particularly relates to a preparation method and application of an oil tea cake extract.
Background
Tea saponin, a natural surfactant, is extracted from camellia seed of camellia of the family camellia. However, at present, the oil tea cake resources are basically used as wastes, and the application way of fully utilizing the oil tea cake resources to develop tea saponin and update tea saponin is one of the important tasks of reasonably utilizing the oil tea cake resources in China at present.
The tea saponin is used as a natural nonionic surfactant, has the surface critical cross-linking concentration (CMC) of 0.5%, the HLB value of 16, extremely small surface tension, two parts of hydrophilicity and lipophilicity, better performance in dispersing, foaming, decontamination and other aspects, and has the advantages of antioxidation, sterilization, anti-inflammation, antipruritic, degradability, no pollution, no toxicity and the like.
However, there are problems in research and application of tea saponin at present, such as: the industrially extracted tea saponin finished product has low yield and purity, and particularly, the oil and fat in the oil tea cake is separated by a multi-step process, the purification technology is improved, and the extraction cost is required to be reasonably reduced.
Therefore, a method for extracting tea saponin from oil tea cake with high yield, few process steps and high purification degree is needed.
Disclosure of Invention
The invention provides a preparation method of an oil tea cake extract, which aims to solve the technical problems of low effect, high extraction cost, poor oil separation effect in oil tea cake and the like in the prior art.
A second object of the present invention is to provide a washing and caring product containing the oil tea cake extract.
In order to achieve the first object, the present invention adopts the following technical scheme:
a preparation method of an oil tea cake extract comprises the following steps:
step 1: pretreating oil tea cakes and meal to obtain tea cake and meal powder;
step 2: preparing a reverse micelle extraction solution;
step 3: placing the pretreated oil tea cake and meal powder into the reverse micelle solution in the step 2, performing ultrasonic extraction and centrifugal separation to obtain supernatant, wherein the supernatant is pre-extract of the reverse micelle;
step 4: adding a buffer solution into the supernatant, and performing back extraction and centrifugal separation to obtain an organic phase and a water phase;
step 5: and (3) performing column chromatography separation on the organic phase to obtain the oil tea cake extract.
The preparation method of the oil tea cake extract comprises the following components in parts by weight: 1-5 parts of surfactant, 10-25 parts of nonpolar organic solvent and 70-90 parts of deionized water.
The preparation method of the oil tea cake extract comprises the following steps of adding a nonpolar organic solvent into an aqueous solution containing a surfactant, and carrying out ultrasonic mixing and dissolution at 30-50 ℃, wherein the reverse micelle solution has W 0 20-40.
The preparation method of the oil tea cake extract comprises the step of preparing the oil tea cake extract, wherein the surfactant is any one of sodium bis (2-ethylhexyl) succinate sulfonate (AOT), cetyl Trimethyl Ammonium Bromide (CTAB) and trioctylmethyl ammonium chloride (TOMAC).
According to the preparation method of the oil tea cake extract, the nonpolar organic solvent is any one of isooctane, cyclohexane, carbon tetrachloride and chloroform.
The preparation method of the oil tea cake extract comprises the steps of crushing, sieving and drying, wherein the drying temperature is 60-80 ℃, and the sieving mesh number is 30-60 meshes.
The preparation method of the oil tea cake extract comprises the step 3, wherein the ultrasonic power is 500-700W.
According to the preparation method of the oil tea cake extract, the buffer solution in the step 4 is a phosphoric acid buffer solution containing KI, and the pH value of the phosphoric acid buffer solution is 7.2-9.8.
The oil tea cake extract obtained by any one of the above preparation methods, wherein the content of tea saponin is 95.1-98.6%, and the oil tea cake extract is used as a washing product.
In order to achieve the second purpose, the invention adopts the following technical scheme:
the detergent comprises the oil tea cake extract as described above, and further comprises the following components in parts by weight: 6-9 parts of sodium dodecyl benzene sulfonate, 2-5 parts of fatty alcohol polyoxyethylene ether sodium sulfate (AES), 10-15 parts of coconut monoethanolamide (6502), 1-2 parts of sodium benzoate, and disodium ethylenediamine tetraacetate (EDTA-Na) 2 ) 0.1-0.3 part, 0.5-1.5 parts of citric acid, 20-30 parts of saturated sodium chloride solution and 40-50 parts of deionized water.
Compared with the prior art, the invention has the following advantages:
1. the invention provides a preparation method of an oil tea cake extract, which is characterized in that a reverse micelle system formed by an aqueous solution containing a surfactant and a nonpolar organic solvent is combined with an ultrasonic method to extract tea saponin in the oil tea cake, and the content of the tea saponin in the obtained oil tea cake extract is greatly improved through front extraction, centrifugation and back extraction, so that the process flow is shortened.
2. The pH value is regulated by the buffer solution, so that the surface charge carried by the polar groups on the surfactant is increased, other impurities in the oil tea cake generate larger static attraction, and impurities such as protein enter reverse micelle groups to separate tea saponin; the reverse micelle system solution is used as the extracting solution, so that the oil and protein in the oil tea cake can be well removed, and the production efficiency is greatly improved.
3. According to the washing and caring product provided by the invention, the oil tea cake extract prepared by the method can be directly used for producing washing and caring products due to the self-contained surfactant, so that the resources are saved, the obtained finished product is rich and dense in foam, the cleaning and decontaminating capability is strong, and the experience demands of consumers are increased.
Detailed Description
The technical scheme of the invention is described below with reference to examples 1-4.
Example 1
Step 1: crushing 100g of oil tea cake to obtain oil tea cake powder, sieving the obtained powder under the condition that the mesh number of the sieve is 30 meshes, and drying the sieved powder at 60 ℃ to obtain crude oil tea cake powder;
step 2: adding isooctane into an aqueous solution containing AOT, and carrying out ultrasonic mixing and dissolution at the temperature of 30 ℃, wherein the obtained solution is clear, namely a reverse micelle extraction solution;
step 3: placing the crude oil tea cake powder into the reverse micelle solution in the step 2, performing ultrasonic auxiliary extraction under the condition that the ultrasonic power is 500W, and performing centrifugal separation on the solution after ultrasonic extraction to obtain supernatant, wherein the supernatant is a pre-extraction solution of the reverse micelle;
step 4: adding a buffer solution containing KI with the pH value of 7.2 into the supernatant, and carrying out back extraction and centrifugal separation to obtain an organic phase and a water phase;
step 5: and (3) performing column chromatography separation on the organic phase to obtain 23.2g of oil tea cake extract.
Example 2
Step 1: crushing 100g of oil tea cake to obtain oil tea cake powder, sieving the obtained powder under the condition that the mesh number of the sieve is 40 meshes, and drying the sieved powder under the condition of 70 ℃ to obtain crude oil tea cake powder;
step 2: adding isooctane into an aqueous solution containing AOT, and carrying out ultrasonic mixing and dissolution at 40 ℃, wherein the obtained solution is clear, namely a reverse micelle extraction solution;
step 3: placing the crude oil tea cake powder into the reverse micelle solution in the step 2, performing ultrasonic auxiliary extraction under the condition that the ultrasonic power is 600W, and performing centrifugal separation on the solution after ultrasonic extraction to obtain supernatant, wherein the supernatant is a pre-extraction solution of the reverse micelle;
step 4: adding a buffer solution containing KI with the pH value of 8.0 into the supernatant, and carrying out back extraction and centrifugal separation to obtain an organic phase and a water phase;
step 5: and (3) performing column chromatography separation on the organic phase to obtain 25.1g of oil tea cake extract.
Example 3
Step 1: crushing 100g of oil tea cake to obtain oil tea cake powder, sieving the obtained powder under the condition that the mesh number of the sieve is 50 meshes, and drying the sieved powder at 70 ℃ to obtain crude oil tea cake powder;
step 2: adding isooctane into an aqueous solution containing AOT, and carrying out ultrasonic mixing and dissolution at 45 ℃, wherein the obtained solution is clear, namely a reverse micelle extraction solution;
step 3: placing the crude oil tea cake powder into the reverse micelle solution in the step 2, performing ultrasonic auxiliary extraction under the condition that the ultrasonic power is 650W, and performing centrifugal separation on the solution after ultrasonic extraction to obtain supernatant, wherein the supernatant is a pre-extraction solution of the reverse micelle;
step 4: adding a buffer solution containing KI with the pH value of 8.7 into the supernatant, and carrying out back extraction and centrifugal separation to obtain an organic phase and a water phase;
step 5: and (3) performing column chromatography separation on the organic phase to obtain 26.8g of oil tea cake extract.
Example 4
Step 1: crushing 100g of oil tea cake to obtain oil tea cake powder, sieving the obtained powder under the condition that the mesh number of the sieve is 60 meshes, and drying the sieved powder at 80 ℃ to obtain crude oil tea cake powder;
step 2: adding isooctane into an aqueous solution containing AOT, and carrying out ultrasonic mixing and dissolution at 50 ℃, wherein the obtained solution is clear, namely a reverse micelle extraction solution;
step 3: placing the crude oil tea cake powder into the reverse micelle solution in the step 2, performing ultrasonic auxiliary extraction under the condition that the ultrasonic power is 700W, and performing centrifugal separation on the solution after ultrasonic extraction to obtain supernatant, wherein the supernatant is a pre-extraction solution of the reverse micelle;
step 4: adding a buffer solution containing KI with the pH value of 9.8 into the supernatant, and carrying out back extraction and centrifugal separation to obtain an organic phase and a water phase;
step 5: and (3) performing column chromatography separation on the organic phase to obtain 28.5g of oil tea cake extract.
Table 1: preparation of reverse micelle solution of examples 1-4 formulation (unit: parts by weight)
The content and purity of tea saponin in the oil tea cake extract in examples 1 to 4 were calculated as shown in Table 2.
Table 2: oil tea cake extract in examples 1-4 and content and purity of tea saponin therein
| Effective component of the product | Example 1 | Example 2 | Example 3 | Example 4 |
| Extract content (g) | 23.2 | 25.1 | 26.8 | 28.5 |
| Tea saponin content (%) | 22.8 | 24.3 | 25.7 | 27.6 |
| Purity of tea saponin (%) | 98.27 | 96.81 | 95.89 | 96.84 |
As can be seen from Table 2, the tea saponin in the oil tea cake is extracted by combining a reverse micelle system with ultrasonic wave, and the content of the tea saponin in the obtained oil tea cake extract is greatly improved by pre-extraction, centrifugation and back extraction, so that the process flow is shortened, compared with the traditional complex and lengthy flow which needs to deoil and degreasing the oil tea cake, the process flow is improved to directly separate the tea saponin, the grease and the protein by using the reverse micelle system, and the electrostatic interaction between the surfactant and the protein and the reverse micelle formed by dissolving the surfactant in a nonpolar organic solvent and enabling the concentration of the surfactant to exceed the critical micelle concentration can lead the tea saponin to be better separated from the grease and the protein, thereby achieving the purification effect, the yield of the tea saponin is higher than 22%, and the purity of the tea saponin is higher than 95.1%.
Example 5 tea saponin application in washing and caring products
Weighing 40 parts of deionized water by taking 5 beakers with the same specification respectively, and weighing 0.2 part of EDTA-Na 2 Adding 8 parts of sodium dodecyl benzene sulfonate slowly into water, stirring slowly, adding 4 parts of AES and 10 parts of 6502 after the sodium dodecyl benzene sulfonate is completely dissolved, stirring for dissolving, adjusting pH=7 by using citric acid, adding 20 parts of saturated sodium chloride solution and 1 part of sodium benzoate, adjusting viscosity to required viscosity, standing for defoaming, adding 0, 20, 30, 40 and 50 parts of oil tea cake extract in the above example 1 respectively until the solution is completely dissolved, marking as numbers 1, 2, 3, 4 and 5, and testing foaming conditions according to national standard GB/T13173-2021 and detergency, as shown in table 3.
Table 3: influence of the addition amount of different oil tea cake extracts on foamability and detergency
As shown in the test results of Table 3, the oil tea cake extract prepared by the method of the invention can be directly used as a washing product due to the self-contained surfactant, has strong bubble capability and high foam density, and has good decontamination effect, and particularly, the detergent prepared by adding 30 parts of the oil tea cake extract has the best effect.
The foregoing description of the preferred embodiments of the present application is not intended to be limiting, but is intended to cover any and all modifications, equivalents, and alternatives falling within the spirit and principles of the present application.
Claims (6)
1. The preparation method of the oil tea cake extract is characterized by comprising the following steps:
step 1: pretreating oil tea cakes and meal to obtain tea cake and meal powder;
step 2: preparing a reverse micelle extraction solution;
step 3: placing the pretreated oil tea cake and meal powder into the reverse micelle solution in the step 2, performing ultrasonic extraction and centrifugal separation to obtain supernatant, wherein the supernatant is pre-extract of the reverse micelle;
step 4: adding a buffer solution into the supernatant, and performing back extraction and centrifugal separation to obtain an organic phase and a water phase;
step 5: separating the organic phase by column chromatography to obtain oil tea cake extract;
the reverse micelle extraction solution in the step 2 comprises the following components in parts by weight: 1-5 parts of surfactant, 10-25 parts of nonpolar organic solvent and 70-90 parts of deionized water;
the surfactant is any one of sodium bis (2-ethylhexyl) succinate sulfonate (AOT), cetyl Trimethyl Ammonium Bromide (CTAB) and trioctylmethyl ammonium chloride (TOMAC);
the nonpolar organic solvent is any one of isooctane, cyclohexane, carbon tetrachloride and chloroform;
the buffer solution in the step 4 is a phosphoric acid buffer solution containing KI, and the pH value of the phosphoric acid buffer solution is 7.2-9.8.
2. The method for preparing the oil tea cake extract according to claim 1, wherein: the preparation method of the reverse micelle solution comprises the following steps of adding a nonpolar organic solvent into an aqueous solution containing a surfactant, and carrying out ultrasonic mixing and dissolution at the temperature of 30-50 ℃, wherein the reverse micelle solution has W 0 20-40.
3. The method for preparing the oil tea cake extract according to claim 1, wherein: the pretreatment in the step 1 comprises the steps of crushing, sieving and drying, wherein the drying temperature is 60-80 ℃, and the mesh number of the sieving is 30-60 meshes.
4. The method for preparing the oil tea cake extract according to claim 1, wherein: the ultrasonic power in the step 3 is 500-700W.
5. The oil tea cake extract prepared by the preparation method of any one of claims 1 to 4, wherein the oil tea cake extract has a tea saponin content of 95.1 to 98.6%, and the oil tea cake extract can be used as a washing product.
6. The detergent comprises the oil tea cake extract as claimed in claim 5, and is characterized by further comprising the following components in parts by weight: 8-11 parts of sodium dodecyl benzene sulfonate, 2-5 parts of fatty alcohol polyoxyethylene ether sodium sulfate (AES), 10-15 parts of coconut monoethanolamide, 1-2 parts of sodium benzoate, and disodium ethylenediamine tetraacetate (EDTA-Na) 2 ) 0.1-0.3 part, 0.5-1.5 parts of citric acid, 20-30 parts of saturated sodium chloride solution and 40-50 parts of deionized water.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102372761A (en) * | 2011-10-10 | 2012-03-14 | 安徽农业大学 | Method for extracting tea saponin from sasanglla cake |
| CN103275163A (en) * | 2013-05-23 | 2013-09-04 | 安徽省华银茶油有限公司 | Extraction method for promoting tea saponin to bleed out through surfactant |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102372761A (en) * | 2011-10-10 | 2012-03-14 | 安徽农业大学 | Method for extracting tea saponin from sasanglla cake |
| CN103275163A (en) * | 2013-05-23 | 2013-09-04 | 安徽省华银茶油有限公司 | Extraction method for promoting tea saponin to bleed out through surfactant |
Non-Patent Citations (2)
| Title |
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| 反胶束萃取法从油茶籽粕提取蛋白与茶油研究;沈杨扬;CNKI 工程科技Ⅰ辑;摘要，第9页 * |
| 超声波- 表面活性剂协同萃取黄姜中 薯蓣皂苷的工艺研究;杨转萍等;《食品科学》;第31卷(第22期);46-49 * |
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