TWI571269B - Extraction method of camellia oleifera abel seed, the extract, and its applications - Google Patents

Description

Extraction method of bitter tea oil mash, extract thereof, and use thereof

The invention relates to extracting camellia seed meal by using a polyol as a solvent, extracting a flavonoid glycoside, a triterpenoid glycoside, and other phenolic substances in the bitter tea seed meal, and extracting the obtained essence. The extract is directly added to the cosmetic without the problem of solvent separation, and the bitter tea oil is well applied. The bitter tea oil extract of the invention can be used for producing various series of products such as bath essence, shampoo, hair lotion, skin lotion, cosmetics and sunscreen lotion.

The extraction of bitter tea oil and tea seed oil is currently based on mechanical pressing, others have solvent methods, and supercritical carbon dioxide extraction methods developed in recent years.

(1) Pressing method: For the traditional method, it can be divided into two methods: cold pressing and hot pressing. The cold pressing method treats bitter tea seeds (large fruit species and small fruit types) or tea seeds into a cake shape, and at normal temperature, oil is pressed, and after precipitation and filtration to remove impurities, the nutrients and the nutrients are retained. Antioxidant golden yellow "cold-pressed bitter tea oil", but its residual oil rate is higher; hot pressing method first bucks bitter tea seeds or tea seeds at about 80 ° C -135 ° C, and then presses oil, its color Deeper.

(2) Solvent method: the tea seed (large fruit and small fruit), tea seed or oil-dried tea simmer is immersed in a solvent (usually n-hexane), and extracted by extraction and solvent removal. If the solvent is not completely removed, the solvent remaining in the oil may not be directly mixed with food or may be consumed without heating because of doubts about health. In the extraction process, the solvent is often dispersed due to the escape of the solvent. Question.

(3) Supercritical carbon dioxide extraction method: It is a relatively advanced production method, which not only has high extraction rate, but also can be directly extracted, no complicated process such as filtration, and no residual solvent. The product retains a variety of nutrients and has the characteristics of high purity and good quality, but the equipment cost is high. The test shows that by using supercritical carbon dioxide to extract the tea stalk which has been prepared by the traditional method, it can be seen that the residual oil remaining in the samovar will be extracted, and the hot pressed samovar can be extracted 8.12%, and after cold pressing The samovar can extract 11.95%.

The extraction of bitter tea oil and tea seed oil is mainly based on mechanical pressing method, but the residual oil rate is high, and after the bitter oil tea seed extract oil, the bitter tea seed oil is mostly used for dish washing and doing. For applications such as soaps that are less economical, it is a pity that the essence of bitter tea oilseeds is not fully utilized.

The invention relates to a method for extracting camellia seed meal by using a polyol as a solvent, and the polyol can easily extract the flavonoid glycoside, the triterpenoid glycoside, and other phenolic substances in the bitter tea seed meal. Extracted, and the polyol itself is a solvent having a moisturizing function and being non-toxic, and the obtained extract can be directly added to the cosmetic without the problem of solvent separation, and the bitter tea oil is well applied, and the method of the present invention And the product is quite industrially useful. The bitter tea oil extract of the invention can be used for producing various series of products such as bath essence, shampoo, hair lotion, skin lotion, cosmetics and sunscreen lotion.

The present invention uses a polyol as an extraction solvent for Camellia oleracea, such as propylene glycol, butylene glycol, glycerin, 2-methyl-1,3-propanediol, dipropylene glycol, polypropylene glycol, dibutyl glycol, Polytetramethylene glycol, 1,2,4-butanetriol, trihydroxymethylpropane, trihydroxymethylethane, sorbitol, mannitol, pentaerythritol, polyether polyol, long-chain polyol, branching Type polyol, Polyethylene glycol and the like are commonly used as moisturizing ingredients in cosmetics. Therefore, the extract can be directly applied to the formulation of cosmetics after being filtered, and the use of polyols does not require the problem of solvent separation. Oil sputum is well applied.

According to previous studies of the present invention, Camellia oleifera is rich in flavonoid glycosides and three types of glycosides, while flavonoids and other phenolic substances have free radical scavenging, anti-inflammatory and anti-cancer functions. It was also confirmed that Camellia oleifera extract can delay the production of conjugated diene and lipid peroxide, and has good DPPH scavenging ability and reducing power. The total phenolic amount of extracts from leaves, flowers and peels of Camellia oleifera is 95 mg (GAE) / g - 135 mg (GAE) / g, wherein the total phenolic amount of the leaves is slightly higher than that of the peel, and the total amount of phenols of the flowers is the least; The inhibitory effect of oxidation shows that the leaf extract has the best antioxidant properties, and the peel is second. If it can be effectively extracted, it is a resource that can be utilized. In addition, Camellia oleifera seed and tea seed hull contain flavonoids, which are tested for their antioxidant activity by DPPH method, showing good free radical scavenging effect and increasing economic benefits.

The invention utilizes a polyol as a solvent to extract the oil tea seed meal, and the polyol can easily extract the essence components such as the flavonoid glycoside, the triterpenoid glycoside, and other phenolic substances in the bitter tea seed meal. However, the bitter tea oil is well applied, and the method and product of the present invention are quite industrially useful.

The method for extracting bitter tea oil of the present invention utilizes a polyol as an extraction solvent of bitter oil tea, wherein the bitter tea oil: solvent is impregnated at a mass ratio of 1:1 to 1:30, and then filtered.

The method for extracting bitter tea oil of the present invention, wherein the polyol is selected from the group consisting of propylene glycol, butylene glycol, glycerin, 2-methyl-1,3-propanediol, dipropylene glycol, polypropylene glycol, dibutyl glycol, Polytetramethylene glycol, 1,2,4-butanetriol, trihydroxymethylpropane, trihydroxymethylethane, sorbitol, mannitol, pentaerythritol, polyether polyol, C ₂ ~ C ₂₀ long chain Any one of a polyol, a C ₂ -C ₂₀ branched polyol, or a polyethylene glycol or a mixture thereof.

The method for extracting bitter tea oil of the present invention, wherein the polyol is preferably selected from the group consisting of: propylene glycol, butylene glycol, glycerin, 2-methyl-1,3-propanediol, or dipropylene glycol or mixture.

The method for extracting bitter tea oil of the present invention, wherein the solvent further comprises ethanol or water in addition to the polyol.

The method for extracting bitter tea oil of the present invention, further comprising extracting the bitter tea oil solution containing the impregnated polyol for extraction.

The method for extracting bitter tea oil of the present invention further comprises extracting the bitter tea oil solution containing the impregnated polyol by microwave heating.

The bitter tea oil extract of the invention can be used for producing various series of products such as bath essence, shampoo, hair lotion, skin lotion, cosmetics and sunscreen lotion.

The shampoo composition of the present invention comprises: an anionic cleansing surfactant of the present invention in an amount ranging from 0.5 to 30% by weight, and an anionic cleansing surfactant in an amount ranging from 0.5 to 45% by weight, in an amount ranging from 0.5 to 40% by weight. The total amount of the co-surfactant (eg, nonionic surfactant), surfactant (including any co-surfactant and/or any emulsifier) in the shampoo composition of the present invention, to the total of the composition The surfactant is usually from 1 to 50% by weight, preferably from 2 to 40% by weight, more preferably from 10 to 30% by weight, based on the total amount of the surfactant. The cationic polymer is usually present in the shampoo composition of the present invention. The total weight is from 0.01 to 15% by weight, preferably from 0.05 to 10% by weight, more preferably from 0.08 to 5% by weight, based on the total of the cationic polymer. The thickener is usually from 0 to 10%, preferably from 0.1 to 6%, based on the total weight of the composition of the shampoo composition of the present invention. More preferably from 0.5 to 2% by weight of all thickeners. The shampoo compositions of the present invention comprise from 50 to 98%, preferably from 60 to 90% by weight, based on the total weight of the composition. The shampoo compositions of the present invention may generally comprise other ingredients, as desired.

In the present invention, the conditioner composition comprises: the content of the bitter tea extract and the cationic surfactant of the present invention in the range of 0.5 to 30% by weight in the range of 0.01 to 10%, preferably 0.05 to 7.5%. Preferably, the cationic surfactant of 0.1 to 5% by weight, the conditioner conditioning composition of the present invention, the fatty alcohol and/or fatty acid is in the range of 0.01 to 10%, preferably 0.1 to 8%, more preferably It is 0.2 to 6%, preferably 0.3 to 5% by weight. The cationic polymer is usually from 0.01 to 15% by weight, preferably from 0.05 to 10% by weight, more preferably from 0.08 to 5% by weight, based on the total weight of the composition, of the total cationic polymer in the conditioning composition of the present invention. The fluorenone is present in the composition of the invention in an amount of from 0.0 to 10%, preferably from 0.05 to 5%, more preferably from 0.5 to 2% by weight, based on the total weight of the composition.

The bath essence composition of the present invention comprises: an anionic cleansing surfactant of the present invention in an amount ranging from 0.5 to 30% by weight, an anionic cleansing surfactant in an amount ranging from 0.5 to 45% by weight, and a content ranging from 0.5 to 40% by weight. The total amount of surfactant (e.g., nonionic surfactant), surfactant (including any co-surfactant and/or any emulsifier) in the bath essence composition of the present invention, based on the total weight of the composition Typically, from 1 to 50% by weight, preferably from 2 to 40% by weight, more preferably from 10 to 30% by weight, based on the total weight of the composition, of all surfactants, cationic polymers, in the bath essence compositions of the present invention. 0 to 5 wt%, preferably 0.05 to 3 wt%, more preferably 0.08 to 2 wt% of all cationic polymers, and in the conditioner of the present invention, the content of the fatty alcohol and/or fatty acid is in the range of 0 to 8%, preferably From 0.05 to 5%, optimally from 0.3 to 3% by weight of fatty alcohols and/or fatty acids. The humectant content ranges from 0 to 20% by weight in the present invention. The thickener is usually from 0 to 10%, preferably from 0.1 to 6%, more preferably from 0.5 to 2% by weight, based on the total weight of the composition, of the total thickener in the bath essence composition of the present invention. The bath essence composition of the present invention comprises from 50 to 98%, preferably from 60 to 90% by weight, based on the total weight of the composition. The bath essence composition of the present invention may generally contain other ingredients as needed.

Examples of suitable anionic cleansing surfactants according to the invention are alkyl sulfates, alkyl ether sulfates, alkyl aryl sulfonates, alkyl hydroxy sulfonates, alkyl succinates, alkyl sulfosuccinates, sulfo groups. Alkyl succinate, N-alkyl sarcosylate, alkyl phosphinate, alkyl ether phosphate, and alkyl ethers and salts thereof, especially sodium, magnesium, ammonium and mono-, di- and triethanolamine salts. The alkyl and sulfhydryl groups typically contain from 8 to 18, preferably from 10 to 16 carbon atoms and may be unsaturated. The alkyl ether sulfate, the alkyl ether sulfosuccinate, the alkyl ether phosphate and the alkyl ether ether and salts thereof may contain from 1 to 20 ethylene oxide or propylene oxide units per molecule.

Typical anionic cleansing surfactants useful in the present invention include sodium sulfonate, ammonium lauryl sulfosuccinate, lauryl sulfate, sodium lauryl ether, sodium sulfosuccinate, lauryl ether, ammonium sulfate lauryl Ester, ammonium sulfate lauryl ether, sodium sulfonate lauryl phenyl ester, sodium sulfonate triethanolamine lauryl phenyl ester, sodium isethionate cocoamate, sodium isethionate lauryl ester, lauryl ether carboxylic acid and Sodium sarcosinate N-lauryl ester.

Preferred anionic cleansing surfactants are sodium lauryl sulfate, sodium lauryl sulfate (n) EO (where n is 1 to 3), sodium sulfo-sodium lauryl ether (n) EO, (where n is 1 to 3) ammonium sulfate lauryl ester, ammonium sulfate lauryl ether (n) EO, (where n is 1 to 3), sodium isethionate cocoa butter and lauryl ether carboxylic acid (n) EO, (where n is 10 to 20 ). Mixtures of any of the foregoing anionic cleansing surfactants are also suitable.

The total amount of anionic cleansing surfactant in the shampoo composition of the present invention, The total range of anionic cleansing surfactants is generally from 0.5 to 45%, preferably from 1.5 to 35%, more preferably from 5 to 20% by weight based on the total weight of the composition.

The co-surfactants described herein assist in providing aesthetic, physical or cleansing of the composition.

Examples of co-surfactants are nonionic surfactants which may be included in the range of from 0.5 to 20%, preferably from 2 to 10% by weight, based on the total weight of the composition.

For example, may be included in representative nonionic surfactant within the bath and shampoo compositions of the present invention fine include aliphatic (C ₈ -C ₁₈₎ of the first or second linear or branched alcohols with ethylene generally A condensation product of ethane and usually having from 6 to 30 ethylene oxide based oxyalkylenes.

Other representative nonionic surfactants include mono or dialkyl alkanolamines. Examples thereof include cocoa mono or diethanol decylamine and cocoa monoisopropanol decylamine.

Other nonionic surfactants which may be included in the shampoo and shower gel compositions of the present invention are alkyl polyglycosides (APGs). Typically, APG is an alkyl group comprising a linker (optionally via a bridging group) to a block of one or more glycosidic groups. Preferably, the APGS is defined by the formula: RO-(G) _n wherein R is a branched or straight chain alkyl group which may be saturated or unsaturated and G is a glycosyl group. R may represent an average alkyl chain length of from about C ₅ to about C ₂₀ . Preferably, R can represent an average alkyl chain length of from about C ₈ to about C ₁₂ . Most preferably, the value of R is between about 9.5 and about 10.5. G may be selected from a C ₅ or C ₆ monosaccharide residue, preferably a glycoside. G may be selected from the group consisting of glucose, xylose, lactose, fructose, mannose, and derivatives thereof. G is preferably glucose. The degree of polymerization n can have a value of from about 1 to about 10 or more. Preferably, the value of n is from about 1.1 to about 2. Most preferably, the value of n is from about 1.3 to about 1.5.

Suitable alkyl polyglycosides for use in the present invention are commercially available and include, for example, The materials were confirmed as: OramiX NS10 ex Seppic; Plantaren 1200 and Plantaren 2000 ex Henkel.

Other sugar-derived nonionic surfactants may interface included in the compositions of the present invention comprises a C ₁₀ -C ₁₈ N- alkyl (C ₁ -C ₆₎ polyhydroxy fatty acid acyl amine, such as C ₁₂ -C ₁₈ N- methyl Reduction of glucosamine, as described in WO 92 06154 and US 5 194 639, and N-alkoxy polyhydroxy fatty acid guanamines, such as C ₁₀ -C ₁₈ N-(3-methoxypropyl) reduced glucosides amine.

Preferred examples of the co-surfactant of the present invention are amphoteric or zwitterionic surfactants, which may be included in an amount ranging from 0.5 to about 20%, preferably from 1 to 10% by weight, based on the total weight of the composition. Within.

Examples of the amphoteric or zwitterionic surfactants of the present invention include alkylamine oxides, alkylbetaines, alkylamidopropyl betaines, alkyl sulfobetaines, and sulphate Esters, alkyl carboxyglycinates, alkyl amphoteric acetates, alkyl amphoteric propionates, alkyl amphoteric glycosides, alkyl guanamidopropyl hydroxy sultaines, decyl tartrates and thioglycolic acid An ester wherein the alkyl group and the fluorenyl group have 8 to 19 carbon atoms. Typical amphoteric and zwitterionic surfactants useful in the shampoos of the present invention include laurylamine oxide, cocodimethyl sulphopropyl betaine, lauryl betaine, cocoapropyl propyl betaine, and cocoa nicotinic acid. sodium.

A particularly preferred amphoteric and zwitterionic surfactant is cocoapropyl propyl betaine.

Mixtures of any of the foregoing amphoteric and zwitterionic surfactants are also suitable. A preferred mixture is a mixture of the cocoamidopropyl betaine and the other amphoteric or zwitterionic surfactants described above. Preferably, the other amphoteric or zwitterionic surfactant is sodium cocoamphoacetate.

The total amount of surfactant (including any co-surfactant and/or any emulsifier) in the shampoo compositions of the present invention, usually from 1 to about the total weight of the composition. 50%, preferably 2 to 40%, more preferably 10 to 30% by weight of all surfactant.

The cationic polymer is a preferred component of the shampoo and bath essence compositions of the present invention for enhanced conditioning properties.

Suitable cationic polymers can be homopolymers which can be substituted cationically or can be formed from two or more monomers. The weight average ( _Mw ) molecular weight of the polymer is typically between 100,000 and 2,000,000 Daltons. The polymer has a cationic nitrogen which comprises groups such as quaternary ammonium or protonated amine groups or mixtures thereof. If the molecular weight of the polymer is too low, the regulation efficiency will be poor. If it is too high, it will have a high tensile viscosity, which will result in the viscosity of the composition when it is poured.

The cationic nitrogen-containing group is usually present as a substituent on the fraction of all the monomer units of the cationic polymer. Thus, when the polymer is not a homopolymer, it may comprise spacer non-cationic monomer units. The polymer is described in the CTFA Cosmetic Ingredient Directory, 3 ^rd edition. The ratio of cationic to non-cationic monomer units is selected to give a polymer having a cationic charge density in the desired range, which is typically from 0.2 to 3.0 meq/gm. The cationic charge density of the polymer is suitably determined by the Kjeldahl method, as described in US Pharmacopoeia, under the chemical test of nitrogen.

Suitable cationic polymers include, for example, ethylene monomers having cationic amine or quaternary ammonium functionality with water soluble spacer monomers such as (meth) acrylamide, alkyl and dialkyl (meth) acrylamide, A copolymer of (meth)acrylic acid alkyl ester, ethylene caprolactone and vinyl pyrrolidine. The alkyl- and dialkyl-substituted monomers preferably have a C ₁ -C ₇ alkyl group, more preferably a C _1-3 alkyl group. Other suitable spacers include vinyl esters, vinyl alcohol, maleic anhydride, propylene glycol, and ethylene glycol.

The cationic amine can be a first, second or third amine, depending on the particular species and pH of the composition. Usually, it is preferred to use the second and third amines, especially the third amine.

The amine-substituted ethylene monomer and amine can be polymerized in the form of an amine and then converted to ammonium by quaternization.

The cationic polymer may comprise a mixture of monomer units derived from amine and/or quaternary ammonium substituted monomers and/or compatible spacer monomers.

Suitable cationic polymers include, for example: - polymers containing cationic diallyl quaternary ammonium including, for example, dimethyl diallyl ammonium chloride homopolymers and acrylamide and dimethyl diallyl ammonium a copolymer of chlorides, known in the industry (CTFA) as Polyquaternium 6 and Polyquaternium 7; a mineral acid salt of an amine-alkyl ester of a copolymer having an unsaturated carboxylic acid having 3 to 5 carbon atoms; (as described in U.S. Patent No. 4,009,256); - a cationic polypropylene decylamine (as described in WO 95/22311).

Other cationic polymers that may be used include cationic polysaccharide polymers such as cationic cellulose derivatives, cationic starch derivatives, and cationic guar gum derivatives.

Cationic polysaccharide polymers suitable for use in the compositions of the present invention include monomers of the formula: AO-[RN ⁺ (R ¹ )(R ² )(R ³ )X ^- ] wherein: A is an anhydroglucose residue, such as Starch or cellulose dehydrated glucose residue. R is an alkylene group, an oxygen-containing alkylene group, a polyoxyalkylene group or a hydroxyalkylene group or a combination thereof. R ¹ , R ² and R ³ each represent an alkyl group, an aryl group, an alkylaryl group, an aralkyl group, an alkoxyalkyl group or an alkoxyaryl group, each group containing up to about 18 carbon atoms. The total number of carbon atoms of each cationic group (i.e., the sum of carbon atoms in R ¹ , R ² and R ³ ) is preferably about 20 or less, and X is an anion counterion.

Another type of cationic cellulose includes polymeric quaternary ammonium salts of hydroxyethyl cellulose reacted with lauryl dimethyl ammonium substituted epoxides, known in the industry (CTFA) as Polyquaternium 24. Such materials are available from A merchol Corp., for example, trade names Polymer LM-200.

Other suitable cationic polysaccharide polymers include those comprising a quaternary nitrogen cellulose ether (for example, as described in U.S. Patent No. 3,962,418), a copolymer of etherified cellulose and starch (for example, as described in U.S. Patent No. 3,958,581).

A particularly suitable type of cationic polysaccharide polymer which can be used is a cationic guar gum derivative such as guar hydroxypropyltrimethylammonium chloride (commercially available from Rhodia Corporation in the JAGUAR trade name series). Examples of such materials are JAGUAR C13S, JAGUAR C14, JAGUAR C15, JAGUAR C17 and JAGUAR C16 Jaguar CHT and JAGUAR C162.

Preferably, the aqueous shampoo and shower gel compositions of the present invention further comprise a thickening agent, the primary function of which is to increase viscosity and moisturize. Selected from: electrolyte, water soluble polymer. The electrolyte is, for example, sodium chloride or ammonium chloride; the water-soluble polymer glue is selected from the group consisting of chitosan, sanxian gum, starch, gum arabic, guar gum, cyclodextrin, margar gum, gelatin, methylol Cellulose, hydroxyethyl cellulose, polyvinylpyrrolidone, polyvinyl alcohol or a mixture thereof, polyacrylic acid, crosslinked polymer of acrylic acid, copolymer of acrylic acid and hydrophobic monomer, copolymerization of carboxylic acid containing monomer and acrylate a crosslinked copolymer of acrylic acid and acrylate, a heteropolysaccharide gel, and a crystalline long chain mercapto derivative. The long chain mercapto derivative is preferably selected from the group consisting of ethylene glycol stearate, an alkanolamine having a fatty acid having 16 to 22 carbon atoms, and a mixture thereof. Ethylene glycol distearate and ethylene glycol distearate 3 are preferred long chain mercapto derivatives because they provide a pearly luster of the composition. Polyacrylic acid is available on the market as Carbopol 420, Carbopol 488 or Carbopol 493. Polymers of acrylic acid crosslinked with a polyfunctional agent can also be used; commercially available as Carbopol 910, Carbopol 934, Carbopol 941 and Carbopol 980. Suitable copolymer of carboxylic acid containing monomer and acrylate An example is Carbopol 1342. All Carbopol (trade name) materials are available from Goodrich.

A suitable crosslinked polymer of acrylic acid and acrylate is Pemulen TR1 or Pemulen TR2. Suitable heteropolysaccharide gums are xanthan gum, for example, available from Kelzan Mu. Mixtures of any of the above thickeners can be used.

The thickener is generally from 0 to 10%, preferably from 0.5 to 6%, more preferably from 0.9 to 2% by weight, based on the total weight of the composition, of all thickeners of the shampoo and essence composition of the present invention.

Another preferred product form of the compositions of the present invention is a conditioning conditioner composition for treating hair (usually after shampooing) and subsequent rinsing.

The conditioner conditioning composition typically comprises one or more conditioning surfactants which are cosmetically acceptable and suitable for topical application to the hair.

Suitable conditioning surfactants include such cationic surfactants selected from those used alone or in combination. Preferably, the cationic surfactant has the formula N ⁺ R ¹ R ² R ³ R ⁴ wherein R ¹ , R ² , R ³ and R ⁴ are each (C ₁ -C ₃₀ )alkyl or benzyl. Preferably, one, two or three of R ¹ , R ² , R ³ and R ⁴ are each (C ₄ to C ₃₀ ) alkyl and the other R ¹ , R ² , R ³ and R ⁴ are (C ₁ to C ₆ )alkyl or benzyl. More preferably, one or two of R ¹ , R ² , R ³ and R ⁴ are each (C ₆ to C ₃₀ ) alkyl and the other R ¹ , R ² , R ³ and R ⁴ are (C ₁ -C ₆ )alkyl or benzyl. The alkyl group may contain one or more ester (-OCO- or -COO-) and/or ether (-O-) linkages within the alkyl chain, as desired. The alkyl group may optionally be substituted by one or more hydroxyl groups. The alkyl group may be a straight chain or a branched chain, and for an alkyl group having 3 or more carbon atoms, it is a cyclic chain. The alkyl group may be saturated or may contain one or more carbon-carbon double bonds (eg, an oil base). The alkyl group is optionally ethoxylated on the alkyl chain with one or more ethyleneoxy groups.

Suitable cationic surfactants for use in the conditioner compositions of the present invention include cetyltrimethylammonium chloride, lanthanum chloride, cetylpyridinium chloride, tetramethylammonium chloride, tetraethylammonium chloride, chlorinated chlorinated Trimethylammonium chloride, dodecyltrimethylammonium chloride, cetyltrimethylammonium chloride, octyldimethylbenzylammonium chloride, decyldimethylbenzylammonium chloride, stearyl dimethyl chloride Benzylammonium, dodecyldimethylbenzylammonium chloride, dioctadecyldimethylammonium chloride, trimethylammonium chloride, dihydrogenated tallow ammonium chloride (eg, Arquad2HT/75, from AkzoNobel) Company), chlorinated cocotrimethylene chloride, chlorinated PEG-2-oleyl ammonium and its corresponding hydroxide. Other suitable cationic surfactants include such materials having CTFA designations Quaternium-5, Quaternium-31, and Quaternium-18. Mixtures of any of the foregoing materials are also suitable. A particularly useful cationic surfactant for use in the conditioning agents according to the present invention is cetyltrimethyl chloride, commercially available, for example, as GENAMIN CTAC, ex Hoechst Celanese. Another particularly useful cationic surfactant for use in the conditioning agents according to the present invention is chloroammonium chloride, commercially available, for example, as GENAMIN KDMP, ex Clariant.

In the conditioning agent of the present invention, the cationic surfactant is present in an amount ranging from 0.01 to 10%, preferably from 0.05 to 7.5%, most preferably from 0.1 to 5% by weight of the composition.

Modulators of the invention are also typically incorporated into fatty alcohols. It is believed that the combination of the fatty alcohol and the cationic surfactant in the conditioning composition is particularly advantageous because it results in the formation of a layered phase in which the cationic surfactant is dispersed.

Representative fatty alcohols and/or fatty acids contain from 8 to 22 carbon atoms, more preferably from 16 to 22 carbon atoms. As the higher alcohol, a linear alcohol having 16 or more carbon atoms is preferably used, and in particular, a linear alcohol having a carbon number of 16 to 22 such as stearyl alcohol, behenyl alcohol, oleyl alcohol, cetyl-stearyl alcohol or cetyl alcohol can be suitably used. , its derivatives and mixtures.

Further, the higher alcohol derivative to which the higher alcohol of the present invention can be used in combination is a compound represented by the following general formula (I). R ¹ -O-(-(CH ₂ ) _y -O-) _x -H(I) In the above general formula (I), R ¹ represents a linear or branched fatty acid residue having 10 to 24 carbon atoms, x And y are integers of 1 or more and 3 or less, respectively. Examples of such a compound include polyoxyethylene (1) stearyl alcohol, polyoxyethylene (2) cetyl-stearyl alcohol, polyoxypropylene (3) lauryl alcohol, polyoxybutylene (2) cetyl alcohol, and the like.

In the case of a higher fatty acid, a compound having a carbon number of 12 to 22 is particularly preferable, and examples thereof include lauric acid, myristic acid, palmitic acid, stearic acid, behenic acid, oleic acid, and undecylenic acid. ), tall oil fatty acid (tall acid), isostearic acid, linoleic acid, linolenic acid, eicosapentaenoic acid , docosahexaenoic acid (DHA, docosahexaenoic acid), coconut oil fatty acid, etc., may be used alone or in combination of two or more. In particular, in the present invention, a linear fatty acid having a carbon number of 16 or more is preferred, and a linear fatty acid having 16 to 22 carbon atoms such as palmitic acid, stearic acid or behenic acid can be suitably used. The use of such materials is also exemplified by the fact that it promotes the overall conditioning characteristics of the compositions of the present invention.

The fatty alcohol and/or fatty acid in the conditioner conditioning composition of the present invention typically ranges from 0.01 to 10%, preferably from 0.1 to 8%, more preferably from 0.2 to 6%, most preferably from 0.3 to 5% by weight of the composition. The weight ratio of the cationic surfactant to the fatty alcohol is suitably from 1:1 to 1:10, preferably from 1:1.5 to 1:8, most preferably from 1:2 to 1:5. If the weight ratio of cationic surfactant to fatty alcohol is too high, this can cause eye irritation from the composition. If it is too low, it can make some consumers feel harsh hair.

The compositions of the present invention may contain other conditioning agents to optimize the wetting and drying conditioning benefits. A particularly preferred regulator is an oxime ketone latex.

Suitable ketone ketones include such oxime ketone formers, for example, polydiorganosiloxanes, especially polydimethyl oxiranes, having a CTFA designation of dimethoxane, a polydihydroxyl group having a hydroxyl end group. Methyl decane having a CTFA designation dimethicone, and an amine functional polydimethyl methoxy alkane having a CTFA label amine dimethyl polyoxy siloxane.

Emulsion droplets may typically have a Sauter (the Sauter) range of mean droplet diameter (D _3,2) is from 0.01 to 20 micrometers in the compositions of the present invention, preferably 0.2 to 10 microns.

Suitable ketone ketones for use in the compositions of the present invention are available from suppliers of ketones such as Dow Corning and GE Silicones. Due to the ease of processing and control of the size of the fluorenone particles, it is preferred to use the preformed fluorenone latex. The preformed fluorenone latex typically additionally comprises a suitable emulsifier such as an anionic or nonionic emulsifier or a mixture thereof, and may be prepared by chemical emulsification such as latex polymerization or by mechanical emulsification using a high shear mixer. Pre-formed fluorenone emulsions having a Sauter average droplet diameter (D3, 2) of less than 0.15 microns are commonly referred to as microemulsions.

Also suitable are oxime ketones in which a particular type of high molecular weight surface-active block copolymer is blended with an oxime emulsion droplet as described in WO 03/094874. In the material, the fluorenone emulsion droplets are preferably formed of the above polydiorganosiloxane. A preferred form of the surface active block copolymer is according to the formula: Wherein the average value of x is 4 or more and the average value of y is 25 or more. Another preferred form of the surface active block copolymer is according to the formula: Wherein the average value of a is 2 or more and the average value of b is 6 or more.

The anthrone is usually present in the conditioner conditioning composition of the present invention in an amount of from 0.0 to 10%, preferably from 0.05 to 5%, more preferably from 0.5 to 2% by weight, based on the total weight of the composition.

The humectant described in the present invention is selected from the group consisting of: glycerin, propylene glycol, butanediol, methyl propylene glycol, hexahexaol, dipropylene glycol, pentanediol, hexanediol, low molecular weight polyethylene glycol, wood A sugar alcohol, an amino acid, a vinyl pyrrolidone carboxylic acid (PCA) and/or a sodium salt thereof, lactic acid, sodium lactate, hyaluronic acid, collagen, or a mixture thereof, is mainly used as a moisturizing agent for skin and hair.

The preservatives described in the present invention are selected from the group consisting of: benzyl alcohol, phenoxyethanol, sodium alkyl urea, p-hydroxybenzoic acid esters, benzoic acid, 1,3-dimethylol-5,5-di Methyl acetylcholine and triclosan are mainly used to inhibit foreign microorganisms.

The compositions of the present invention may contain additional ingredients for enhanced performance and/or consumer acceptance. The ingredients include fragrances, dyes and pigments, pH adjusters, pearlizers or sunscreens, viscosity modifiers, preservatives and natural hair nutrients such as botanicals, fruit extractants, sugar derivatives, amino acids, silk proteins, Oil, ultraviolet absorber, metal ion blocking agent, pH adjuster, skin and hair nutrient, vitamins, oxidation inhibitor, oxidation prevention aid, etc.

Fig. 1 Photograph of the extract of the present invention (A) solvent impregnation; (B) filtrate.

Figure 2 FTIR of the bitter tea oil extract of the present invention; (A) extraction with different solvents at room temperature; (B) single solvent extraction at room temperature; (C) extraction with different solvents under microwave.

Fig. 3 UV-VIS absorption spectrum of the bitter tea oil extract of the present invention (A) The room temperature extract is diluted 100 times; (B) The microwave extract is diluted 100 times.

Hereinafter, the present invention will be described in detail based on examples, but the present invention is not limited thereto.

Preparation of extract of bitter tea oil

The present invention respectively uses water (abbreviated as W), ethanol (abbreviated as E), propylene glycol (abbreviated as PG), butanediol (abbreviated as BG), glycerol (glycerol, abbreviated as G), sorbitol, polyethylene glycol and The mixture was used as an extraction solvent for the extraction of bitter tea oil.

Refer to Table 1 for an experimental ratio table for extracting bitter tea oil from various solvents of the present invention.

Example 1

(take the No. 1 extract in Table 1 as an example)

The extraction steps are as follows:

1. The mechanically pressed bitter tea oil cake is ground into a fine powder with a sickle.

2. Weigh 40 g of the above-mentioned bitter tea oil fine powder, add a mixed solvent of 40 g of ethanol (abbreviated as E) and 80 g of propylene glycol, carry out microwave for 30 seconds, cool for 5 minutes, and repeat 3 times.

3. After cooling to room temperature, filter and place the filtrate in a freezer for later use.

After step 1-3, the different solvents and microwave conditions are sequentially changed, and the extraction experiments of Nos. 2 to 19 are carried out, and the photograph of the obtained extract is as shown in the first figure: (A) solvent impregnation; (B) filtrate, It is shown that the extraction of glycerol (G) is the best for the bitter tea oil. It can dissolve the bitter tea oil into a paste, the darkest color, followed by propylene glycol and butanediol; the water has the worst solubility, followed by alcohol. The extracts all showed a light color.

Determination of the properties of bitter tea oil extract

1. Determination of FTIR functional groups, determination of extracted components.

2. The UV-visible spectrophotometry (Ultraviolet- visible spectroscopy, UV- Vis) absorbance was measured the ability of the extract.

The second figure (A) (B) (C) shows the FTIR of the bitter tea oil extract of the present invention; (A) extraction with different solvents at room temperature; (B) single solvent extraction at room temperature; (C) microwave Extracted under different solvents, It is characterized by flavonoid glycosides, triterpenoid glycosides, and polyphenols at 2020-2240nm, 1460, 1237, and 1051nm. 920-940, 840-850nm shows flavonoid glycosides, triterpenoids. The fingerprint absorption of the glycoside flavonoid glycoside and the triterpenoid glycoside shows that the present invention extracts the bitter tea oil sputum by using the polyol, and can effectively extract the essential components and fully apply them. Free radicals, anti-inflammatory and anti-cancer functions are also very suitable for skin and hair care products.

The third figure shows the UV-VIS absorption spectrum of the bitter tea oil extract of the present invention (A) the room temperature extract is diluted 100 times; (B) the microwave extract is diluted 100 times, which shows that it is very strong at a wavelength of 200-400 nm. The absorption, especially at 230 nm, has a strong absorption at 280-400 nm, which shows that the extract of the method of the invention has strong absorption to both UVA and UVB segments, and is suitable as a sunscreen product and microwave extraction. Can extract more sunscreen ingredients.

Shampoo formula

Among them, the extract (3-EG) extract extract No. 3, the solvent is ethanol (E) and glycerin (G); (5-PG) extract extract No. 5, the solvent is propylene glycol.

Modulation method:

(1) D-panthenol and Glycerin are first weighed into a 250mL beaker, stirred evenly with a glass rod, and then weighed into other beakers and stirred evenly.

(2) Add the B raw materials and mix well.

The shampoo composition containing the bitter tea oil extract of the invention is quite clean, moisturized, moisturized, silky and not tangled.

Run Conditioner Composition Formula

Among them, the extract (6-BG) surface extract No. 6, the solvent is butanediol; (7-G) surface extract No. 7, the solvent is glycerin.

Modulation method:

Heat each of (A) and (B) to 70-80 ° C, then add (A) to the fully melted (B), stir to emulsifie, add to (C) when cooled to 40 ° C, continue to stir evenly , cooled to room temperature. The moisturizing conditioner composition containing the bitter tea oil extract is relatively easy to rinse, moisturize, moisturize, silky and not tangled. Camellia oleifera is rich in flavonoid glycosides and three types of glycosides, while flavonoids and other phenolic substances have free radical scavenging, can delay the production of conjugated diene and lipid peroxide, and have good DPPH clearance. The ability, the antioxidant and the reducing power, therefore, the bitter tea extract of the present invention has a very good protective effect on the hair.

Bath essence formula

Among them, the extract (2-EB) surface extract No. 2, the solvent is ethanol (E) and butanediol (B); (5-PG) surface extract No. 5, the solvent is propylene glycol.

Modulation method:

Weigh all the raw materials of (A) together and mix well. The bath essence product containing the bitter tea oil extract is relatively clean, moisturizing, moisturizing, good in touch and not tight. Camellia oleifera is rich in flavonoid glycosides and three types of glycosides, while flavonoids and other phenolic substances have free radical scavenging, can delay the production of conjugated diene and lipid peroxide, and have good DPPH clearance. The ability, antioxidant and reducing power, therefore, the bitter tea extract of the present invention has a very good protective effect on the skin.

Industrial availability

The polyol extracting of the bitter tea oil of the present invention can effectively extract the flavonoid glycoside, the triterpenoid glycoside, the polyphenols, and the like of the essential components, and fully apply them.

The polyol of the invention extracts bitter tea oil sputum, which can effectively increase the moisturizing ability of shampoo, hair lotion and beauty care products.

The polyol extracting of the bitter tea oil of the invention can effectively increase the sunscreen ability of the chemical sunscreen agent, and can greatly reduce the use amount of the chemical sunscreen agent, and reduce the toxicity and side effects of the sunscreen agent.

The bitter tea oil extract of the invention can be used for producing shampoo, shower gel, hair lotion, skin cream, cosmetics, sunscreen and the like.

While the present invention has been described above in terms of several preferred embodiments, it is not intended to limit the present invention, and any one of ordinary skill in the art can make any changes without departing from the spirit and scope of the invention. The scope of the present invention is defined by the scope of the appended claims.

Claims (9)

The invention relates to an extraction method of bitter tea oil scorpion, which uses polyhydric alcohol as an extraction solvent of bitter oil tea stalk, wherein, bitter tea oil mash: solvent is impregnated at a mass ratio of 1:1 to 1:30, and then filtered, and the obtained extract liquid is obtained. Directly applied without solvent separation, wherein the polyol is selected from the group consisting of: butanediol, glycerol, 2-methyl-1,3-propanediol, dipropylene glycol, dibutylene glycol, 1,2,4-butyl Any one of triol, trimethylolpropane, trihydroxymethylethane, sorbitol, mannitol, pentaerythritol, and mixtures thereof. The method for extracting bitter tea oil according to claim 1, wherein the polyol is selected from the group consisting of: butanediol, glycerin, 2-methyl-1,3-propanediol, or dipropylene glycol or Its mixture. The method for extracting bitter tea oil according to claim 1, wherein the solvent further comprises ethanol or water in addition to the polyol. The method for extracting bitter tea oil according to claim 1 , further comprising extracting the bitter tea oil solution containing the polyol by heating generally or by microwave. An extract of the bitter tea oil mash, which is obtained by the extraction method of the bitter tea mash according to any one of claims 1 to 4, and the obtained extract is directly applied without solvent separation. A shampoo composition comprising: an anionic cleansing surfactant having a content ranging from 0.5 to 30% by weight, as described in claim 5, an anionic cleansing surfactant having a content ranging from 0.5 to 45% by weight, in a range of 0.5 To 40% by weight of the co-surfactant, the content is in the range of 0.01 to 15% by weight of the cationic polymer, the thickening agent in the range of 0.1 to 10% by weight, and 50 to 98% by weight of water. A conditioner conditioner composition comprising: a content range of 0.5 to 30% by weight, such as a patent application A bitter tea oil extract according to item 5, a cationic surfactant having a content ranging from 0.01 to 10% by weight, a fatty alcohol and/or a fatty acid in an amount ranging from 0.01 to 10% by weight, and a cationic polymer of from 0.01 to 15% by weight. A bath essence composition comprising: an anionic cleansing surfactant having a content ranging from 0.5 to 30% by weight, as described in claim 5, an anionic cleansing surfactant having a content ranging from 0.5 to 45% by weight, in a range of from 0.5 to 40% by weight of a co-surfactant, a humectant in an amount ranging from 0 to 20% by weight, a thickener in an amount ranging from 0.1 to 10% by weight, and a water in a range of from 50 to 98%. The invention relates to the use of the extract of bitter tea oil as described in claim 5, which is used as a formula for shampoo, shower gel, hair care lotion, skin cream, cosmetics and sunscreen lotion.