CN116332894A - Method for preparing cocoa extract and cosmetic - Google Patents
Method for preparing cocoa extract and cosmetic Download PDFInfo
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- CN116332894A CN116332894A CN202310293896.6A CN202310293896A CN116332894A CN 116332894 A CN116332894 A CN 116332894A CN 202310293896 A CN202310293896 A CN 202310293896A CN 116332894 A CN116332894 A CN 116332894A
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- 229940119429 cocoa extract Drugs 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 42
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- 230000005684 electric field Effects 0.000 claims abstract description 70
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- 239000000243 solution Substances 0.000 claims abstract description 48
- 239000000843 powder Substances 0.000 claims abstract description 46
- 239000002608 ionic liquid Substances 0.000 claims abstract description 36
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims abstract description 33
- 238000000605 extraction Methods 0.000 claims abstract description 22
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- KWIUHFFTVRNATP-UHFFFAOYSA-O N,N,N-trimethylglycinium Chemical compound C[N+](C)(C)CC(O)=O KWIUHFFTVRNATP-UHFFFAOYSA-O 0.000 claims abstract description 10
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- CWEZAWNPTYBADX-UHFFFAOYSA-N Procyanidin Natural products OC1C(OC2C(O)C(Oc3c2c(O)cc(O)c3C4C(O)C(Oc5cc(O)cc(O)c45)c6ccc(O)c(O)c6)c7ccc(O)c(O)c7)c8c(O)cc(O)cc8OC1c9ccc(O)c(O)c9 CWEZAWNPTYBADX-UHFFFAOYSA-N 0.000 description 11
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- XFZJEEAOWLFHDH-UHFFFAOYSA-N (2R,2'R,3R,3'R,4R)-3,3',4',5,7-Pentahydroxyflavan(48)-3,3',4',5,7-pentahydroxyflavan Natural products C=12OC(C=3C=C(O)C(O)=CC=3)C(O)CC2=C(O)C=C(O)C=1C(C1=C(O)C=C(O)C=C1O1)C(O)C1C1=CC=C(O)C(O)=C1 XFZJEEAOWLFHDH-UHFFFAOYSA-N 0.000 description 7
- MOJZMWJRUKIQGL-FWCKPOPSSA-N Procyanidin C2 Natural products O[C@@H]1[C@@H](c2cc(O)c(O)cc2)Oc2c([C@H]3[C@H](O)[C@@H](c4cc(O)c(O)cc4)Oc4c3c(O)cc(O)c4)c(O)cc(O)c2[C@@H]1c1c(O)cc(O)c2c1O[C@@H]([C@H](O)C2)c1cc(O)c(O)cc1 MOJZMWJRUKIQGL-FWCKPOPSSA-N 0.000 description 7
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- OEIJRRGCTVHYTH-UHFFFAOYSA-N Favan-3-ol Chemical compound OC1CC2=CC=CC=C2OC1C1=CC=CC=C1 OEIJRRGCTVHYTH-UHFFFAOYSA-N 0.000 description 3
- CITFYDYEWQIEPX-UHFFFAOYSA-N Flavanol Natural products O1C2=CC(OCC=C(C)C)=CC(O)=C2C(=O)C(O)C1C1=CC=C(O)C=C1 CITFYDYEWQIEPX-UHFFFAOYSA-N 0.000 description 3
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- 238000002481 ethanol extraction Methods 0.000 description 2
- 238000000338 in vitro Methods 0.000 description 2
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- 239000003960 organic solvent Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 description 2
- 230000036556 skin irritation Effects 0.000 description 2
- 231100000475 skin irritation Toxicity 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- YAPQBXQYLJRXSA-UHFFFAOYSA-N theobromine Chemical compound CN1C(=O)NC(=O)C2=C1N=CN2C YAPQBXQYLJRXSA-UHFFFAOYSA-N 0.000 description 2
- PFTAWBLQPZVEMU-DZGCQCFKSA-N (+)-catechin Chemical compound C1([C@H]2OC3=CC(O)=CC(O)=C3C[C@@H]2O)=CC=C(O)C(O)=C1 PFTAWBLQPZVEMU-DZGCQCFKSA-N 0.000 description 1
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 description 1
- OYHQOLUKZRVURQ-NTGFUMLPSA-N (9Z,12Z)-9,10,12,13-tetratritiooctadeca-9,12-dienoic acid Chemical compound C(CCCCCCC\C(=C(/C\C(=C(/CCCCC)\[3H])\[3H])\[3H])\[3H])(=O)O OYHQOLUKZRVURQ-NTGFUMLPSA-N 0.000 description 1
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- 108010059892 Cellulase Proteins 0.000 description 1
- 241000282412 Homo Species 0.000 description 1
- 238000012404 In vitro experiment Methods 0.000 description 1
- 244000241838 Lycium barbarum Species 0.000 description 1
- 235000015459 Lycium barbarum Nutrition 0.000 description 1
- 241000219071 Malvaceae Species 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- 102000035195 Peptidases Human genes 0.000 description 1
- 108091005804 Peptidases Proteins 0.000 description 1
- JPYHHZQJCSQRJY-UHFFFAOYSA-N Phloroglucinol Natural products CCC=CCC=CCC=CCC=CCCCCC(=O)C1=C(O)C=C(O)C=C1O JPYHHZQJCSQRJY-UHFFFAOYSA-N 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- 238000000692 Student's t-test Methods 0.000 description 1
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- 235000005487 catechin Nutrition 0.000 description 1
- ADRVNXBAWSRFAJ-UHFFFAOYSA-N catechin Natural products OC1Cc2cc(O)cc(O)c2OC1c3ccc(O)c(O)c3 ADRVNXBAWSRFAJ-UHFFFAOYSA-N 0.000 description 1
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- 238000004140 cleaning Methods 0.000 description 1
- 229940110456 cocoa butter Drugs 0.000 description 1
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- 238000001914 filtration Methods 0.000 description 1
- -1 flavanol oligomers Chemical class 0.000 description 1
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- 239000000796 flavoring agent Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 235000013355 food flavoring agent Nutrition 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
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- 230000005764 inhibitory process Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
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- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
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- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
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- QCDYQQDYXPDABM-UHFFFAOYSA-N phloroglucinol Chemical compound OC1=CC(O)=CC(O)=C1 QCDYQQDYXPDABM-UHFFFAOYSA-N 0.000 description 1
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- 238000000638 solvent extraction Methods 0.000 description 1
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- 239000008117 stearic acid Substances 0.000 description 1
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- 210000002536 stromal cell Anatomy 0.000 description 1
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- 238000001521 two-tailed test Methods 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/58—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4
- C07D311/60—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2
- C07D311/62—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2 with oxygen atoms directly attached in position 3, e.g. anthocyanidins
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/49—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
- A61K8/4973—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with oxygen as the only hetero atom
- A61K8/498—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with oxygen as the only hetero atom having 6-membered rings or their condensed derivatives, e.g. coumarin
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
- A61K8/9783—Angiosperms [Magnoliophyta]
- A61K8/9789—Magnoliopsida [dicotyledons]
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/007—Preparations for dry skin
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/08—Anti-ageing preparations
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B61/00—Dyes of natural origin prepared from natural sources, e.g. vegetable sources
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0096—Purification; Precipitation; Filtration
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
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- General Health & Medical Sciences (AREA)
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- Public Health (AREA)
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- Birds (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
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- Gerontology & Geriatric Medicine (AREA)
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Abstract
The application relates to the field of cosmetics, and relates to a method for preparing a cocoa extract and a cosmetic. The method for preparing cocoa extract comprises subjecting the mixture of cocoa powder and extractive solution to high-voltage pulsed electric field treatment to obtain treated solution; extracting the treatment fluid; obtaining procyanidine, wherein the content of procyanidine is not less than 0.58mg/mL; the extracting solution is an aqueous solution of ionic liquid according to mass percent; the mass concentration of the extracting solution is 20-50%; the ionic liquid comprises: 15-30% of betaine; 60-84.5% of glycerol; propylene glycol 0.5-10%; the electric field strength of the high-voltage pulse electric field is 1 kV/cm-8 kV/cm. According to the scheme, the cocoa powder is extracted by adopting the ionic liquid and is cooperated with the high-voltage pulse electric field, so that the content of procyanidine in the cocoa extract is improved while the extraction by adopting the natural extracting solution is ensured, the method is more suitable for industrial application and is more suitable for being used in cosmetics.
Description
Technical Field
The application relates to the field of cosmetics, in particular to a method for preparing a cocoa extract and a cosmetic.
Background
Cocoa (Theobroma cacao) belongs to the genus Malvaceae, and is known as a three-major beverage crop with coffee, tea. The use of cocoa can be traced to a long-term age, and the congress of crown ceremony and religious beliefs in the period of the Aztec empire are said to occur, and both the father and the noble will be the sincere to drink a liquid extracted from the cocoa tree as a gift to be given to humans by the emperor. Cocoa beans are seeds of the cocoa tree that are rich in oleic acid, linoleic acid, stearic acid, organic matter, minerals, polymeric tannins, theobromine, flavonoids, and other active ingredients. The product has good moisturizing effect, and can help to lock skin moisture. The cocoa also has remarkable oxidation resistance and can delay the aging of skin.
Currently, cocoa extract has been used in cosmetics, chinese patent CN202110154930.2 discloses the use of cocoa extract in the preparation of anti-aging and tumor-inhibiting drugs, revealing that cocoa extract promotes tumor inhibition by targeted action on tumor microenvironment, eliminating senescent cells, and by eliminating senescent stromal cells. Chinese patent CN201711300916.9 discloses whitening and moisturizing cream containing the extract of the Brazilian cocoa, and the whitening and moisturizing active ingredient obtained by compounding the extract of the Bacilian cocoa and the polysaccharide of the matrimony vine according to a specific proportion has obvious synergy in whitening, moisturizing and moisturizing. Chinese patent CN201110067951.7 discloses a method for preparing cocoa extract, which uses cellulase, pectase and proteinase with strong specificity as catalyst to make biodegradation, then uses solvent to make two-step extraction, and adopts membrane separation technology to make normal-temp. refining of extract so as to obtain the invented high-concentration cocoa flavouring agent.
In general, there are cosmetics containing cocoa extracts on the market at present, and the preparation modes of cocoa extracts are different, but the disadvantages of low preparation efficiency, poor efficacy and the like in the preparation process are generally existed.
Disclosure of Invention
An object of embodiments of the present application is to provide a method of preparing a cocoa extract, a cosmetic.
In a first aspect, the present application provides a method of preparing a cocoa extract comprising:
carrying out high-voltage pulse electric field treatment on the mixed solution of the cocoa powder and the extracting solution to obtain a treatment solution;
extracting the treatment fluid; obtaining procyanidine, wherein the content of procyanidine is not less than 0.58mg/mL;
the extracting solution is an aqueous solution of ionic liquid according to mass percent; the mass concentration of the extracting solution is 20-50%;
the ionic liquid comprises: 15-30% of betaine; 60-84.5% of glycerol; propylene glycol 0.5-10%;
the electric field strength of the high-voltage pulse electric field is 1 kV/cm-8 kV/cm.
According to the scheme, the cocoa powder is extracted by adopting the ionic liquid and is cooperated with the high-voltage pulse electric field, so that the content of procyanidine in the cocoa extract is improved while the extraction by adopting the natural extracting solution is ensured, and the method is more suitable for industrial application and more suitable for being used in cosmetics. According to the scheme, the ionic liquid containing betaine, glycerol and propylene glycol is adopted, and the formula of the ionic liquid is limited in the proportion range, so that the content of procyanidine can be effectively increased. Furthermore, the extraction content of procyanidine in the cocoa powder can be not lower than 0.58mg/mL by adopting the ionic liquid extraction and cooperating with the high-voltage pulse electric field with the electric field strength of 1 kV/cm-8 kV/cm.
In the prior art, water or other single solvents are usually adopted to extract cocoa powder, however, the content of procyanidine in the cocoa extract obtained by adopting the water to extract the cocoa powder is very low, and ethanol and the like are adopted to extract, although the content of procyanidine in the cocoa extract can be improved, the ethanol extraction has potential safety hazards, is not suitable for industrial application (ethanol is strictly forbidden in a workshop in part of areas), and the cocoa extract is extracted by adopting the ethanol and the like, so that the non-natural extractant is applied to cosmetics and can possibly generate risks of skin irritation and the like.
In other embodiments of the present application, the ionic liquid comprises, in mass percent:
betaine 16-29%; 61-80% of glycerol; 0.6-10% of propylene glycol.
In other embodiments of the present application, the mass concentration of the extraction solution is 30% -45%.
In other embodiments of the present application, the mixing ratio of cocoa powder to extract in the mixture is: (1 g-10 g): (15 mL-100 mL).
In other embodiments of the present application, the high-voltage pulsed electric field treatment of the mixture of cocoa powder and extract comprises:
performing high-voltage pulse electric field treatment on the mixed solution of cocoa powder and extracting solution, wherein the high-voltage pulse electric field treatment comprises the following steps:
and treating the mixed solution by adopting a high-voltage pulse electric field with the electric field strength of 1 kV/cm-8 kV/cm.
In other embodiments of the present application, the high-voltage pulsed electric field treatment of the mixture of cocoa powder and extract comprises:
and treating the mixed solution by adopting a high-voltage pulse electric field with the electric field strength of 4 kV/cm-8 kV/cm.
In other embodiments of the present application, the number of times of high-voltage pulse electric field treatment is performed on the mixed solution of cocoa powder and extract is selected from 10 times to 100 times.
In other embodiments of the present application, the high-voltage pulsed electric field treatment of the mixture of cocoa powder and extract comprises:
and treating the mixed solution for 10 to 100 times by adopting a high-voltage pulse electric field with the electric field strength of 4 to 8kV/cm.
In a second aspect, the present application provides a cosmetic comprising a cocoa extract produced by the method of producing a cocoa extract provided in the first aspect.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present application and therefore should not be considered limiting the scope, and that other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a standard curve drawn with procyanidine concentration on the abscissa and absorbance on the ordinate.
Detailed Description
For the purposes of making the objects, technical solutions and advantages of the embodiments of the present application more clear, the technical solutions in the embodiments of the present application will be clearly and completely described below, and it is obvious that the described embodiments are some embodiments of the present application, but not all embodiments.
Thus, the following detailed description of the embodiments of the present application is not intended to limit the scope of the application, as claimed, but is merely representative of selected embodiments of the application. All other embodiments, which can be made by one of ordinary skill in the art based on the embodiments herein without making any inventive effort, are intended to be within the scope of the present application.
The inventor finds that the cocoa butter in the cocoa has a lubricated texture, a small plasticity range, a melting point close to human skin and very easy to be melted and absorbed, and is a good hydrating humectant and lubricant. Therefore, the moisturizing cream has good moisturizing effect, can moisten dry and water-deficient skin well, and prevents peeling and cracking. In addition, the cocoa has rich polyphenol substances, so the cocoa has remarkable oxidation resistance and free radical removal capability, can delay skin aging, and helps to prevent and remove wrinkles. Cocoa-enriched polyphenols, mainly flavanol oligomers, have higher content of flavanol substances in cocoa than most other foods, including procyanidins and monomeric catechin, wherein procyanidins are polyphenols with relatively strong activity in cocoa, and cocoa powder is conventionally extracted by using single solvent such as water, ethanol, etc. as extractant, and has lower content of active substances, especially procyanidins.
Embodiments of the present application provide a method of preparing a cocoa extract, comprising:
carrying out high-voltage pulse electric field treatment on the mixed solution of the cocoa powder and the extracting solution to obtain a treatment solution;
extracting the treatment fluid; obtaining procyanidine, wherein the content of procyanidine is not less than 0.58mg/mL;
the extracting solution is an aqueous solution of ionic liquid according to mass percent; the mass concentration of the extracting solution is 20-50%;
the ionic liquid comprises: 15-30% of betaine; 60-84.5% of glycerol; propylene glycol 0.5-10%;
the electric field strength of the high-voltage pulse electric field is 1 kV/cm-8 kV/cm.
According to the scheme, the cocoa powder is extracted by adopting the ionic liquid and is cooperated with the high-voltage pulse electric field, so that the content of procyanidine in the cocoa extract is improved while the extraction by adopting the natural extracting solution is ensured, and the method is more suitable for industrial application and more suitable for being used in cosmetics. According to the scheme, the ionic liquid containing betaine, glycerol and propylene glycol is adopted, and the formula of the ionic liquid is limited in the proportion range, so that the content of procyanidine can be effectively increased. Furthermore, the extraction content of procyanidine in the cocoa powder can be not lower than 0.58mg/mL by adopting the ionic liquid extraction and cooperating with the high-voltage pulse electric field with the electric field strength of 1 kV/cm-8 kV/cm. According to the scheme, the cocoa powder is extracted by adopting the ionic liquid and is cooperated with the high-voltage pulse electric field, so that the content of procyanidine in the cocoa extract is improved while the extraction by adopting the natural extracting solution is ensured, and the method is more suitable for industrial application and more suitable for being used in cosmetics.
In the prior art, water or other single solvents are usually adopted to extract cocoa powder, however, the content of procyanidine in the cocoa extract obtained by adopting the water to extract the cocoa powder is very low, and organic solvents such as ethanol are adopted to extract, although the content of procyanidine in the cocoa extract can be improved, the ethanol extraction has potential safety hazards, is not suitable for industrial application (ethanol is strictly forbidden in a workshop in partial areas), and the cocoa extract is extracted by adopting the ethanol and the like, so that the non-purely natural extractant is applied to cosmetics and can possibly generate risks of skin irritation and the like.
In some embodiments of the present application, a method of preparing a cocoa extract comprises the steps of:
and S1, preparing a mixed solution of cocoa powder and an extracting solution.
Further, in some embodiments of the present application, the cocoa powder described above may be selected from cocoa powder or natural cocoa powder.
Further, in some embodiments of the present application, the mixing ratio of the cocoa powder in the mixed solution and the extracting solution is: (1 g-10 g): (15 mL-100 mL).
Further, in some embodiments of the present application, the mixing ratio of the cocoa powder in the mixed solution and the extracting solution is: (1 g-10 g): (15 mL-80 mL).
Further alternatively, in some embodiments of the present application, the mixing ratio of the cocoa powder in the mixed liquor and the extract is: (1.5 g-9.5 g): (15.5 mL-50 mL).
Illustratively, in some embodiments of the present application, the mixing ratio of cocoa powder to extract in the mixture is: 2g:16mL, 3g:17mL, 4g:18mL, 5g:20mL, 8g:23mL, 10g:25mL, 11g:26mL.
Further alternatively, in some embodiments of the present application, when cocoa powder may be selected from the cocoa powder described above, the cocoa powder may be prepared by pulverizing the cocoa beans. Illustratively, the cocoa powder is obtained by comminuting using a high-speed breaker.
Further, in some embodiments of the present application, the ionic liquid comprises, in mass percent:
betaine 16-29%; 61-80% of glycerol; 0.6-10% of propylene glycol.
Illustratively, in some embodiments of the present application, the ionic liquid includes, in mass percent:
betaine 16%, 17%, 18%, 19%, 20%, 21%, 22%, 23%, 24%, 25%, 26%, 27%, 28%, or 29%;
61%, 62%, 65%, 68%, 70%, 72%, 75%, 78%, 80% glycerol;
propylene glycol 0.6%, 0.8%, 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9% or 10%.
Further, in some embodiments of the present application, the mass concentration of the above-mentioned extracting solution is 30% to 50%.
Further alternatively, in some embodiments of the present application, the concentration of the above-described extract is 31% to 49% by mass.
Illustratively, the extract has a mass concentration of 31%, 32%, 35%, 38%, 40%, 42%, 45%, 48%, or 49%.
Further, in some embodiments of the present application, the step of preparing the above-mentioned extracting solution includes mixing the ionic liquid with water to obtain an aqueous solution of the ionic liquid.
Further, in some embodiments of the present application, the mass concentration of the aqueous solution of the prepared ionic liquid is 30% to 50%.
Further, in some embodiments of the present application, the mixing of the cocoa powder with the extract comprises:
mixing cocoa powder with the aqueous solution of the ionic liquid, and stirring uniformly.
Further alternatively, when the cocoa powder is mixed with the aqueous solution of the ionic liquid prepared by the method, the ratio of feed to liquid is controlled: (1 g-10 g): (15 mL-100 mL).
And S2, performing high-voltage pulse electric field treatment on the mixed solution of the cocoa powder and the extracting solution to obtain a treatment solution.
Further, in some embodiments of the present application, the electric field strength of the high-voltage pulsed electric field is 1kV/cm to 8kV/cm.
The electric field intensity of the high-voltage pulse electric field is limited to be 1 kV/cm-8 kV/cm, so that the cell perforation effect on the cocoa beans can be improved, the larger the leaching amount of the active ingredient is, the stronger the efficacy of the active ingredient is, the active ingredient of the procyanidine cannot be damaged in the range, and the efficacy of the active ingredient of the procyanidine is ensured; has more powerful effect on extracting procyanidine, and is beneficial to improving the extraction quantity of procyanidine.
When the electric field intensity of the high-voltage pulse electric field is lower than the lower limit of the range, the perforation effect on cocoa cells is reduced, the dissolution amount of the active ingredients is reduced, and the efficacy of the active ingredients is reduced because the electric field intensity is too low; when the electric field intensity of the high-voltage pulse electric field is higher than the upper limit of the range, the procyanidine active ingredient is damaged, and the efficacy of the procyanidine active ingredient is reduced. The method creatively adopts the high-voltage pulse electric field technology to break the cell walls of the cocoa beans, so that the functional components in the cocoa beans are fully released, the cocoa extract with strong efficacy is obtained, the high-voltage pulse electric field technology is applied to the preparation process of the cocoa extract, a certain reference is provided for efficient extraction of the functional components in the cocoa beans, and a new direction is developed for the application of the technology.
Further alternatively, in some embodiments of the present application, the electric field strength of the high-voltage pulsed electric field is 1.1kV/cm to 7.9kV/cm.
Illustratively, in some embodiments of the present application, the electric field strength of the high-voltage pulsed electric field is:
1.2kV/cm, 1.5kV/cm, 2.0kV/cm, 2.5kV/cm, 3.0kV/cm, 3.5kV/cm, 4kV/cm, 4.5kV/cm, 5kV/cm, 5.5kV/cm, 6kV/cm, 6.5kV/cm, 7kV/cm or 7.5kV/cm.
In other embodiments of the present application, the high-voltage pulsed electric field treatment of the mixture of cocoa powder and extract comprises:
and treating the mixed solution by adopting a high-voltage pulse electric field with the electric field strength of 4 kV/cm-8 kV/cm.
Further, in some embodiments of the present application, the high-voltage pulsed electric field treatment of the mixed solution of cocoa powder and extract comprises:
and treating the mixed solution for 10-100 times by adopting a high-voltage pulse electric field with the electric field strength of 1-8 kV/cm to obtain the treatment solution.
Further alternatively, in some embodiments of the present application, the mixed solution is treated 11 to 90 times with a high-voltage pulsed electric field having an electric field strength of 1kV/cm to 8kV/cm to obtain a treated solution.
The mixed solution is treated with a high-voltage pulse electric field having an electric field strength of 1kV/cm to 8kV/cm for 12 times, 15 times, 20 times, 25 times, 30 times or 50 times, to obtain a treated solution.
And step S3, extracting the treatment liquid obtained in the step S2.
Further, in some embodiments of the present application, extracting the treatment fluid includes:
and (3) leaching the treatment liquid obtained in the step (S2) at 20-30 ℃ for 10-60 min.
Further optionally, in some embodiments of the present application, extracting the treatment fluid includes:
and (3) leaching the treatment liquid obtained in the step (S2) at the temperature of 21-29 ℃ for 11-59 min.
Illustratively, extracting the treatment fluid includes:
the treatment solution obtained in the step S2 is leached at 20 ℃ for 20min, or the treatment solution obtained in the step S2 is leached at 25 ℃ for 15min, or the treatment solution obtained in the step S2 is leached at 30 ℃ for 10min, or the treatment solution obtained in the step S2 is leached at 21 ℃ for 30min.
And S4, compounding the filtrate obtained after the extraction in the step S3 with polyalcohol.
Further, in some embodiments of the present application, the polyol comprises: at least one of glycerin or pentanediol.
Illustratively, in some embodiments of the present application, the above-described polyol is selected from glycerol, pentanediol, or a mixture of glycerol and pentanediol. Further alternatively, when the above polyol is a mixture of glycerin and pentanediol, the above glycerin and pentanediol are compounded in an arbitrary mass ratio.
Further, in some embodiments of the present application, the compounding of the filtrate obtained after the extraction in the step S2 with the polyol includes:
compounding the filtrate and the polyol according to the mass ratio of (1-10) to (40-50).
Further alternatively, in some embodiments of the present application, the compounding of the filtrate obtained after the extraction in the step S2 with the polyol includes:
compounding the filtrate and the polyol according to the mass ratio of (1-9) to (41-49).
Illustratively, the filtrate obtained after the extraction in the step S2 is compounded with a polyol, including:
the filtrate and the polyalcohol are compounded according to the mass ratio of 1:50, 2:49, 3:46, 4:47, 5:46, 6:45, 7:42 or 8:41.
Some embodiments of the present application provide a cosmetic comprising a cocoa extract produced by the method of producing a cocoa extract provided in any of the previous embodiments.
The method creatively adopts the high-voltage pulse electric field technology to break the cell walls of the cocoa beans, so that the functional components in the cocoa beans are fully released, the cocoa extract with strong efficacy is obtained, the high-voltage pulse electric field technology is applied to the preparation process of the cocoa extract, a certain reference is provided for efficient extraction of the functional components in the cocoa beans, and a new direction is developed for the application of the technology.
Furthermore, the ionic liquid is used as an extraction solvent to be cooperated with a high-voltage pulse electric field technology, so that the solubility can be improved, the stability can be enhanced, the environment-friendly and safe advantages are realized, and the defect that an organic solvent is difficult to remove is avoided.
Further, the ionic liquid adopted by the application has the moisturizing effect, and the ionic liquid is adopted as the extracting agent to help enhance the moisturizing effect of the cocoa extract.
The features and capabilities of the present application are described in further detail below in connection with the examples:
the method for preparing the cocoa extract comprises the following steps:
(1) Preparing cocoa powder: preparing commercially available natural cocoa powder;
(2) Mixing ionic liquid with water to prepare ionic liquid aqueous solution; the specific proportion of the ionic liquid is shown in table 2;
(3) Preparing cocoa extract: adding the cocoa powder prepared in the step (1) into an ionic liquid aqueous solution according to the feed liquid ratio shown in table 2, treating for multiple times by adopting a high-voltage pulse electric field, extracting at room temperature, filtering, collecting filtrate, and mixing the filtrate with glycerol and pentanediol to obtain the cocoa extract. The individual process parameters are shown in Table 1.
And (II) detecting.
The procyanidine content in the cocoa extracts prepared in each example and comparative example was examined using procyanidine content as an index. The cocoa extracts prepared in the examples and comparative examples were examined for moisturizing effect and moisturizing rate. The detection results are shown in Table 3.
1. The method for testing the content of procyanidine comprises the following steps:
determining the content of procyanidins by a vanillin-hydrochloric acid method:
(1) Principle of experiment
The vanillin-hydrochloric acid method has specificity to the reaction of procyanidine, and has better measuring effect on flavanol substances. The principle of the vanillin-hydrochloric acid method is that resorcinol or phloroglucinol on the ring A structure can be condensed with vanillin based on the higher chemical activity of the procyanidine ring A, the product forms colored carbanion under the action of concentrated acid, the absorbance of the product is measured at 497.5nm, and the procyanidine content in the sample can be obtained according to a standard curve. Hydrochloric acid or sulfuric acid can be used as a catalyst in the reaction process.
(2) Reagent preparation
A:1% vanillin solution: accurately weighing 1.000g of vanillin, dissolving in methanol, and fixing the volume to 100mL;
b:8% hydrochloric acid solution: dissolving 8mL of concentrated hydrochloric acid in methanol, and fixing the volume to 100mL;
color-developing agent: the reagent A and the reagent B are prepared according to the proportion of 1:1, and the reagent A and the reagent B are prepared in situ.
(3) Experimental procedure
Accurately weighing a proper amount of procyanidine standard substance, dissolving with methanol to prepare procyanidine standard solution with concentration of 1.2mg/mL, respectively sucking 1, 2, 3, 4 and 5mL, and then fixing volume to 10mL with methanol. 1mL of each of the above-mentioned materials was taken, 5mL of the color-developing agent was added, and the materials were shaken well and protected from light. Maintaining in constant temperature water bath at 30+ -1deg.C for 30min, and maintaining the temperature for colorimetric. The cuvette was taken out, its absorbance was measured at 497.5nm wavelength, procyanidine concentration was plotted on the abscissa, and absorbance value was plotted on the ordinate, and a standard curve was drawn (see fig. 1 of the specification).
The samples of each example and comparative example were diluted in the same ratio, and 1mL of the sample was aspirated to determine absorbance, and the procedure was the same as that of the standard curve. Three replicates were measured for each sample with the sample solvent as a blank. The procyanidin content (concentration) of each of the examples and comparative examples was obtained by conversion according to a standard curve (fig. 1). The results of the procyanidin content of each example and comparative example are shown in Table 3.
2. The method for testing the in-vitro moisturizing effect comprises the following steps:
(1) Principle of in vitro experiments
The method comprises the steps of using a glass plate stuck with a 3M adhesive tape as a carrier, uniformly coating components or products on the surface of the adhesive tape, putting the adhesive tape in a constant temperature and humidity dryer, weighing the mass of a sample at regular time, and calculating the moisture retention rate of the sample.
(2) Specific experimental method
About 0.25g (accurate to 0.0001 g) of each of the examples and comparative examples was weighed and coated on a 3M tape-coated glass plate, the mass M of the 3M tape-coated glass plate and the mass M0 after the coating of the sample were accurately recorded, and the glass plate and the coated sample were placed in a desiccator (relative humidity: 48%) containing a saturated solution of potassium carbonate, and the recorded data mt were weighed and stored for 2, 4, 8, and 24 hours, and the moisture retention rate at this time was calculated. The mean and standard deviation were calculated in triplicate. 10% glycerol (raw material number RE 002) was used as positive control and water as negative control.
The moisture retention rate was calculated as follows: moisture retention (%) = (mt-m)/(m 0-m) ×100%
The results of the in vitro moisturizing rates of the examples and comparative examples are shown in Table 3.
3. The test method of the clinical moisturizing effect comprises the following steps:
(1) Test instrument
(2) Test environment
Environmental conditions: temperature: 21.0 ℃ +/-1.0 ℃; humidity: 50% ± 10%
(3) Test flow
Samples of each example and comparative example were given to 10 subjects, respectively.
1) Any product (cosmetic or external medicine) cannot be used 2-3 days before the test of the tested part, and water cannot be contacted for 1-3 hours. Prior to the test, the subject needs to clean the two-handed forearm inner test uniformly. The cleaning method is to wipe clean with dry facial tissues. The inner sides of the forearms of the two hands of the subject are marked with measuring areas, the areas of the measuring areas are at least 3cm multiplied by 3cm, the same arm can mark a plurality of areas at the same time, and the interval between each measuring area is at least 1cm.
The test should be allowed to sit still for at least 20min in a room meeting the standard before the official test, and water and beverage cannot be drunk. The forearm is exposed, placed in a test condition, and left relaxed.
2) Subject data collection was scheduled before and after 2 hours and 4 hours of use, each time skin parameters were collected using a skin test instrument.
3) Statistical analysis is performed by using Excel and SPSS software, the change of data before and after the test sample is used by a subject is analyzed, and a conclusion is made whether the test sample is effective or not according to the calculation result.
(4) Data analysis method
Descriptive statistics are performed on the measured values of each test area, including number, mean, standard deviation, minimum, median, maximum, and the like. And calculating the difference between the initial value of each test area and the measured value of other time points, and then utilizing the difference to statistically analyze the difference between the product area and the blank control area at different time points.
If the test data are normally distributed, adopting a t-test method to carry out statistical analysis; if the test data are in non-normal distribution, adopting a rank sum test method to carry out statistical analysis.
The statistical methods all use a two-tailed test with a test level α=0.05.
5. Result determination
Positive results: the moisture content of the horny layer in the test area is obviously different before and after the product is used, which indicates that the tested sample has the moisturizing effect.
Negative results: the moisture content of the horny layer in the test area has no significant difference before and after the product is used, which indicates that the tested sample has no moisturizing effect.
The results of the moisturizing effect of the human bodies of each example and comparative example are shown in Table 3.
TABLE 1
TABLE 2
TABLE 3 Table 3
As can be seen from the experimental data, the cocoa extracts prepared in the examples of the present application all have a high procyanidin content, above 0.58mg/mL. The cocoa extract prepared in the comparative example has lower procyanidine content than the examples herein.
Further, as can be seen from the above experimental data, the cocoa extracts prepared in the various examples of the present application have excellent moisturizing effects.
Example 1 it can be seen that conventional aqueous extracts of cocoa have a lower procyanidin content compared to comparative example 1.
Example 1 it can be seen that the conventional butylene glycol extraction method has a lower procyanidin content of the cocoa extract compared to comparative example 3.
Example 1 it can be seen that the conventional propylene glycol extraction method cocoa extract has a lower procyanidin content compared to comparative example 3.
From this, it can be demonstrated that the conventional single solvent extraction method has a low procyanidin content of the cocoa extract.
As can be seen from the comparison of example 1 and comparative example 2, the procyanidine content of the cocoa extract is greatly improved by adopting the synergistic combination of the ionic liquid solution and the high-voltage pulse electric field treatment.
In addition, the ionic liquid extracting solution has all raw material components of pure natural substances, and is more mild and non-irritating when used for preparing cosmetics.
The foregoing description is only of the preferred embodiments of the present application and is not intended to limit the same, but rather, various modifications and variations may be made by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principles of the present application should be included in the protection scope of the present application.
Claims (10)
1. A process for preparing a cocoa extract comprising:
carrying out high-voltage pulse electric field treatment on the mixed solution of the cocoa powder and the extracting solution to obtain a treatment solution;
extracting the treatment liquid to obtain procyanidine, wherein the content of procyanidine is not lower than 0.58mg/mL;
the extracting solution is an aqueous solution of ionic liquid according to mass percent; the mass concentration of the extracting solution is 20% -50%;
the ionic liquid comprises: 15-30% of betaine; 60-84.5% of glycerol; propylene glycol 0.5-10%;
the electric field strength of the high-voltage pulse electric field is 1 kV/cm-8 kV/cm.
2. The method for preparing cocoa extract according to claim 1, wherein,
the ionic liquid comprises the following components in percentage by mass:
betaine 16-29%; 61-80% of glycerol; 0.6-10% of propylene glycol.
3. The method for preparing cocoa extract according to claim 1, wherein,
the mass concentration of the extracting solution is 30% -45%.
4. The method for preparing cocoa extract according to claim 1, wherein,
the mixing proportion of the cocoa powder and the extracting solution in the mixed solution is as follows: (1 g-10 g): (15 mL-100 mL).
5. The method for preparing a cocoa extract according to any of the claims 1-4,
the high-voltage pulse electric field treatment of the mixed solution of the cocoa powder and the extracting solution comprises the following steps:
treating the mixed solution by adopting a high-voltage pulse electric field with the electric field strength of 1 kV/cm-8 kV/cm;
optionally, the high-voltage pulse electric field treatment on the mixed solution of the cocoa powder and the extracting solution comprises the following steps:
treating the mixed solution by adopting a high-voltage pulse electric field with the electric field strength of 4 kV/cm-8 kV/cm;
optionally, the times of carrying out the high-voltage pulse electric field treatment on the mixed solution of the cocoa powder and the extracting solution are selected to be 10-100 times.
6. The method for preparing cocoa extract according to claim 1, wherein,
the extracting the treatment fluid comprises the following steps:
leaching for 10 min-60 min at 20-30 ℃.
7. The method for preparing cocoa extract according to claim 1, wherein,
the method further comprises the steps of:
and (3) compounding the filtrate obtained after extraction with polyalcohol.
8. The method for preparing cocoa extract of claim 7,
the polyol comprises: at least one of glycerin or pentanediol.
9. The method for preparing cocoa extract of claim 7,
the step of compounding the filtrate obtained after extraction with polyol comprises the following steps:
and (3) compounding the filtrate and the polyol according to the mass ratio of (1-10) to (40-50).
10. Cosmetic comprising the cocoa extract produced by the process for producing a cocoa extract of any one of claims 1 to 9.
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