CN108096074A - A kind of snake oil composition and preparation method thereof, purposes - Google Patents

A kind of snake oil composition and preparation method thereof, purposes Download PDF

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Publication number
CN108096074A
CN108096074A CN201711455356.4A CN201711455356A CN108096074A CN 108096074 A CN108096074 A CN 108096074A CN 201711455356 A CN201711455356 A CN 201711455356A CN 108096074 A CN108096074 A CN 108096074A
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snake oil
snake
oil
refined
oil composition
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CN108096074B (en
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谢静红
蔡衡
周华锋
周建青
吴姗姗
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Carlyle Cosmetics Co ltd
Crowley Cosmetics Co ltd
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JIANGSU LONGLIQI BIOTECHNOLOGY CO Ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/92Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
    • A61K8/925Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of animal origin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K35/00Medicinal preparations containing materials or reaction products thereof with undetermined constitution
    • A61K35/56Materials from animals other than mammals
    • A61K35/58Reptiles
    • A61K35/583Snakes; Lizards, e.g. chameleons
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/92Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
    • A61K8/922Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
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    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/02Pretreatment
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/10Production of fats or fatty oils from raw materials by extracting
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B3/00Refining fats or fatty oils
    • C11B3/001Refining fats or fatty oils by a combination of two or more of the means hereafter
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B5/00Preserving by using additives, e.g. anti-oxidants
    • C11B5/0021Preserving by using additives, e.g. anti-oxidants containing oxygen
    • C11B5/0028Carboxylic acids; Their derivates
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B5/00Preserving by using additives, e.g. anti-oxidants
    • C11B5/0021Preserving by using additives, e.g. anti-oxidants containing oxygen
    • C11B5/0035Phenols; Their halogenated and aminated derivates, their salts, their esters with carboxylic acids
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B5/00Preserving by using additives, e.g. anti-oxidants
    • C11B5/0085Substances of natural origin of unknown constitution, f.i. plant extracts

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Abstract

The invention discloses a kind of snake oil composition and preparation method thereof, purposes, the snake oil composition includes the following raw material:40 99 parts by weight of refined snake oil, 0.01 0.5 parts by weight of 1 58 parts by weight of assistant formation agent, 0.01 10 parts by weight of antioxidant and plants essential oil, snake oil content is high in the snake oil composition of the present invention, the effect of maximumlly effectively playing snake oil, the snake oil composition is applied to face cream, it is easy to skin absorption, the moisture of skin can be significantly improved, makes skin more lubricious glossy.

Description

A kind of snake oil composition and preparation method thereof, purposes
Technical field
The invention belongs to daily cosmetics fields, and in particular to a kind of snake oil composition and preparation method thereof, purposes.
Background technology
Snake oil is the fat constituent of snake, is a kind of traditional pure natural skin care item, without any side effects to human body and bad Reaction, wherein containing unrighted acids such as linoleic acid, leukotrienes, unrighted acid is the important component of sebum film, Important cytoplasm between horn cell is together constituted with ingredients such as NMF, ceramides, other active components is conducted, has formed Whole skin barrier is a key factor of skin health.Snake oil has stronger affinity and permeability to mucocutaneous, Easily it is absorbed by the skin, the unrighted acid of wherein high-content is the key that it is repaired skin, keeps skin health, and containing big The active skull cap components and antipathogenic composition of amount, therefore snake oil can be used for physical therapy to scald and nurse one's health dry, more wrinkles, rough skin. Unsaturated fatty acid content is higher in snake oil, and skin effect is better, due in snake oil unrighted acid be oxidized easily and It is rotten, each component in snake oil product is not adjusted rationally so that snake oil stability is poor, and adds that snake oil fishy smell is big etc. to ask Topic causes snake oil content in snake oil product to be less than 40%, and content is low, and helper component addition is more so that in snake oil skin care item Snake oil cannot effectively play the effect of snake oil.
A kind of snake oil hand cream as disclosed in Chinese patent literature CN102895167A, contains snake oil 20%-30%, glycerine 15%-20%, chamomile Essence 1%-3%, jojoba oil 1%-3%, safflower seed oil 0.5%-1%, dormant oil 0.2%- 0.5%, cetostearyl alcohol 0.2%-0.5%, sorbierite 0.2%-0.5%, sheep placenta elite 0.2%-0.5%, laruyl alcohol sulphur Acid esters sodium 0.5%-2%, cyclohexasiloxane 0.2%-0.5%, essence 0.2%-0.5%, remaining is medical ventolin.Above-mentioned Main component is vaseline in snake oil hand cream, and snake oil content is only 20%~30%, and is with the addition of other a variety of auxiliary elements, Snake oil snake oil in hand lotion is caused only to play booster action, fails to maximize the effect of effectively playing snake oil.
The content of the invention
Therefore, the technical problem to be solved in the present invention in snake oil product in the prior art is overcome snake oil stability it is poor, Fishy smell is big, can not improve snake oil content in snake oil product, causes the effect of snake oil fails effectively to play snake oil in snake oil product, from And provide snake oil composition that a kind of stability is good, snake oil content without fishy smell is high and preparation method thereof, purposes.
The present invention provides a kind of snake oil composition, including the following raw material:Refined snake oil 40-99 parts by weight, assistant formation Agent 1-58 parts by weight, antioxidant 0.01-10 parts by weight and plants essential oil 0.01-0.5 parts by weight.
The snake oil composition, including the following raw material:80 parts by weight of refined snake oil, 35 parts by weight of assistant formation agent resist 0.3 parts by weight of 5 parts by weight of oxidant and plants essential oil.
The snake oil composition, the refined snake oil are refined liquid snake oil;Preferably, in the liquid snake oil not The mass percent of saturated fatty acid is 70-90%.
The snake oil composition, the assistant formation agent are snake oil saturated fatty acid, other animal or plant sources One or more of mixtures of saturated fatty alcohol, polyunsaturated fatty acid ester or wax.
Preferably, the snake oil saturated fatty acid is solid-state snake oil;Preferably, saturated fatty acid in the solid-state snake oil Mass percent is 50-80%
The snake oil composition, the preparation method of the refined snake oil include the following steps:
(1) snake oil fat granule is taken to be pre-processed;
(2) snake oil fat granule pretreated in step (1) is added in low boiling point organic solvent, while adds in adsorbent And antioxidant, under room temperature shear agitation, filtering remove the low boiling point organic solvent in gained filtrate, obtain snake oil;
(3) snake oil in step (2) is added in low boiling point organic solvent and freezed, separation of solid and liquid obtains filtrate and consolidates Body object, removal low boiling point organic solvent obtain liquid snake oil crude product and solid-state snake oil crude product;
(4) the liquid snake oil crude product and solid-state snake oil crude product that are obtained in step (3) are subjected to decoloration deodorization respectively.
The snake oil composition, in the step (2), the low boiling point organic solvent is n-hexane, ether, ethyl alcohol Or at least one of acetone;The adsorbent is at least one of atlapulgite, aluminium oxide, silica gel or activated carbon;It is described Antioxidant is at least one of citric acid, vitamin C, carnosic acid or tea polyphenols;Preferably, the low boiling point is organic molten Agent is n-hexane;Preferably, the adsorbent is atlapulgite;Preferably, the antioxidant is carnosic acid.
The snake oil composition, in the step (2), the shear agitation step is with rotating speed 200-10000rmp Then shear agitation 0.5-10min stirs 0.5-2h under air-proof condition with rotating speed 200-1000rmp.
The snake oil composition, in the step (2), by the filtrate, rotary evaporation in vacuo is gone at 20-40 DEG C Except low boiling point organic solvent.
The snake oil composition, in the step (2), the addition of the adsorbent is the pretreated snake The 1-30% of the quality of oil and fat grain.
The snake oil composition, in the step (2), the low boiling point organic solvent and the pretreated snake Oil and fat grain mass ratio is (3-10): 1.
The snake oil composition, in the step (2), the addition of the antioxidant is described pretreated The 0.01-0.1% of snake oil fat granule quality.
The snake oil composition in the step (1), takes snake oil fat granule, is immersed in containing antioxidant and chlorine Change sodium pretreatment fluid in, stir 2-5h, repeat impregnate until fat lump without apparent color, it is drained and standby.
Preferably, in step (1), used antioxidant is aqueous citric acid solution.Preferably, the pretreatment fluid The mass concentration of middle citric acid is 0.01-0.05%.Preferably, the mass concentration of citric acid is 0.01%.
Preferably, in step (1), the mass concentration of sodium chloride is 0.1-2% in the pretreatment fluid.Preferably, chlorine The mass concentration for changing sodium is 0.7%.
Preferably, in step (1), the snake oil fat granule is freezing snake oil fat granule or fresh snake oil fat granule. Preferably, snake oil fat granule is fresh snake oil fat granule.
Preferably, in step (1), the snake oil fat granule of 2-15 parts by weight is taken to impregnate the pretreatment of 6-45 parts by volume In liquid, impregnated in the case where temperature is 0-25 DEG C.
In step (3), the snake oil that step (2) extracts is mixed with low boiling point organic solvent for the snake oil composition It closes, freezes 20-30h at -10~0 DEG C, filtrate and solids is then obtained by filtration, respectively at rotary evaporation in vacuo at 30-40 DEG C Low boiling point organic solvent is removed up to liquid snake oil crude product and solid-state snake oil crude product.Preferably, in step (3), the snake oil Mass ratio with low boiling point organic solvent is 1: 1-3.
Preferably, in step (3), the step of further freezing the solids of gained is further included, i.e., by the solid-state Snake oil crude product is mixed with low boiling point organic solvent, is placed in -5~0 DEG C of environment and is freezed 40-50h, separation of solid and liquid, by consolidating for acquisition Body object rotary evaporation in vacuo at 30-40 DEG C removes low boiling point organic solvent, obtains solid-state snake oil crude product.Preferably, in step (3) in, the mass ratio of the solids and low boiling point organic solvent is 1: 1-3.
The snake oil composition, the liquid snake oil crude product for respectively obtaining step (3) in step (3) and solid-state snake Oily crude product is through supercritical CO2Extract decoloration deodorization.
The snake oil composition, unrighted acid in the liquid snake oil in step (3) after decoloration deodorization Mass percent for 70-90%, the solid-state snake oil fusing point is 45-60 DEG C, the matter of saturated fatty acid in the solid-state snake oil Amount percentage is 50-80%.
Preferably, the supercritical CO2Extraction step is as follows, is respectively placed in liquid snake oil crude product and solid-state snake oil crude product It is extracted in extraction kettle, extraction temperature is 30-40 DEG C, extracting pressure 15-45Mpa, flow 20-60L/h, the pressure of separating still For 8-25Mpa, separating still temperature is 30-40 DEG C, after extracting system stablizes 5min, discharges initially-separate snake in clean separation kettle Oil collects snake oil in separating still every 1h, respectively obtains the liquid snake oil and the solid-state snake oil.
The snake oil composition, the antioxidant are tocopherol, sesame seed oil, forulic acid, tea polyphenols or rosemary At least one of extract.
The snake oil composition, the plants essential oil be Rosa Damascana, Lavender or Rosemary Oil in extremely Few one kind.
The present invention provides a kind of methods for preparing the snake oil composition, include the following steps:
1) raw material is weighed according to formula;
2) assistant formation agent is heated to melting, stops heating, added in the refined snake oil and stir evenly;
3) 60-70 DEG C is cooled to, the antioxidant and the plants essential oil is added in, stirs evenly;
4) 50-55 DEG C is cooled to, filling, cooling.
The snake oil composition prepared the present invention provides the snake oil composition or the method is preparing drug, day With the purposes in terms of chemical products.Preferably, the purposes, the daily chemical product are skin protection cosmetics.Preferably, institute The purposes stated, the skin protection cosmetics be for face with, hand with or the face cream of body, cold cream, skin care oil, skin care stick or Facial treatment essence liquid.
Technical solution of the present invention has the following advantages that:
1st, snake oil composition provided by the invention, including the following raw material:Refined snake oil 40-99 parts by weight, assistant formation agent 1-58 parts by weight, antioxidant 0.01-10 parts by weight and plants essential oil 0.01-0.5 parts by weight.In snake oil composition, aid in into Type agent makes to facilitate storage and carrying, antioxidant avoids the unrighted acid in snake oil in solid-state under snake oil composition room temperature Oxidation, the smell that plants essential oil adjusts snake oil composition play the effect of auxiliary skin care, pass through said components and snake oil simultaneously Under coordinated, the stability of the snake oil of acquisition is high, and fishy smell is low, and then can improve the content of snake oil in composition to 37%- 99%, maximumlly effective the effect of playing snake oil, the snake oil composition is applied to face cream, is easy to skin absorption, it can To significantly improve the moisture of skin, make skin more lubricious glossy.
2nd, snake oil composition provided by the invention refines snake oil as refined liquid snake oil, wherein unrighted acid Mass percent is 70-90%, and unsaturated fatty acid content is high, and effect is good.
3rd, the preparation method of refined snake oil provided by the invention, includes the following steps:(1) snake oil fat granule is taken to be located in advance Reason;(2) pretreated snake oil fat granule in step (1) is added in low boiling point organic solvent, while adds in adsorbent and resist Oxidant, under room temperature shear agitation, filtering, removes the low boiling point organic solvent in gained filtrate, obtains snake oil;(3) will Snake oil in step (2), which is added in low boiling point organic solvent, to be freezed, and separation of solid and liquid obtains filtrate and solids, removes low boiling Point organic solvent obtains liquid snake oil crude product and solid-state snake oil crude product;(4) the liquid snake oil crude product that will be obtained respectively in step (3) Decoloration deodorization is carried out with solid-state snake oil crude product.Preparation method provided by the invention by snake oil fat granule pre-process after, with adsorbent, Shear agitation after low boiling point organic solvent and antioxidant mixing, low boiling point organic solvent extraction snake oil, and the suction in mixed liquor Attached dose significantly can carry out decoloration deodorization under low boiling point organic solvent effect to the snake oil extracted, while can be by snake oil The residues adsorption and sedimentation such as remaining albumen in fat granule, beneficial to separation of solid and liquid, antioxidant can avoid snake oil fat in extraction process Fat grain aoxidizes, and the saturated fatty acid in snake oil, which is precipitated, in freezing processing becomes solid-state, and snake oil is separated into liquid by freezing processing Then state snake oil crude product and solid-state snake oil crude product carry out snake oil crude product decoloration deodorization processing, obtained refined snake oil decoloration is de- Taste effect is good, and stability is high.
4th, the preparation method of refined snake oil provided by the invention, by filtrate, rotary evaporation in vacuo removal is low at 20-40 DEG C Boiling point organic solvent, organic solvent boiling point is relatively low, easily removes, and the temperature of rotary evaporation in vacuo removal is kept away between 20-40 DEG C Exempt from snake oil during high temperature to aoxidize.
5th, the preparation method of refined snake oil provided by the invention, snake oil fat is immersed in containing antioxidant and sodium chloride Pretreatment fluid in, stir 2-5h, repeat impregnate until fat lump without apparent color, drained and standby, antioxidant avoids snake oil Fat granule aoxidizes in soaking process, is immersed in sodium-chloride water solution, can be by the water-soluble object such as blood in snake oil fat granule Matter soaking and washing is clean, removes its water-soluble smell of blood.
6th, the preparation method of refined snake oil provided by the invention, the snake oil of extraction is mixed with low boiling point organic solvent, -10 20-30h is freezed at~0 DEG C, filtrate and solids is then obtained by filtration, it is low respectively at rotary evaporation in vacuo removal at 30-40 DEG C The solids with low boiling point organic solvent is mixed up to liquid snake oil crude product, is placed in -5~0 DEG C of environment by boiling point organic solvent Middle freezing 40-50h, separation of solid and liquid, by the solids of acquisition, rotary evaporation in vacuo removal low boiling point is organic molten at 30-40 DEG C Agent obtains solid-state snake oil crude product, and being precipitated the saturated fatty acid in snake oil by freezing processing becomes solid-state, and snake oil is separated into Liquid snake oil crude product and solid-state snake oil crude product can be used for rationally adjusting snake oil composition.
7th, the preparation method of refined snake oil provided by the invention, using supercritical CO2Decoloration deodorization is carried out to snake oil crude product Processing obtains refined snake oil, and decoloration deodorization effect is good, and stability is high, advantageously reduces the acid value and peroxide value of snake oil.
Specific embodiment
Illustrate embodiments of the present invention below by way of specific embodiment, unless otherwise stated, disclosed in this invention Experimental method using the art routine techniques, used reagent and raw material can be bought by market in embodiment.
Embodiment 1
A kind of preparation method of refined snake oil is present embodiments provided, is included the following steps:
(1) the fresh snake oil fat granules of 2kg is taken to be soaked in 10L and contain the citric acid and mass concentration that mass concentration is 0.01% In pretreatment fluid for 0.7% sodium chloride, temperature is to stir 4h at 15 DEG C, is repeated 3 times rear drained and standby;
(2) weigh pretreated snake oil fat granule 1kg in step (1) and 100g atlapulgites, 6kg n-hexanes and 0.5g citric acids are uniformly mixed, and after rotating speed 5000rmp shear agitations 3min, 1h is stirred with rotating speed 800rmp under air-proof condition Afterwards, filtered with G4 sand core funnels, the n-hexane at 35 DEG C in rotary evaporation in vacuo removal filtrate obtains snake oil;
(3) snake oil in step (2) is added in n-hexane and freezed, the mass ratio of snake oil and n-hexane is 1: 2, -5 25h separation of solid and liquid is freezed at DEG C and obtains filtrate and solids, rotary evaporation in vacuo removes n-hexane up to liquid snake oil at 35 DEG C Crude product mixes the solids with n-hexane, and the mass ratio of the solids and n-hexane is 1: 2, is placed in -3 DEG C of environment 45h is freezed, separation of solid and liquid, rotary evaporation in vacuo removes n-hexane at 35 DEG C by the solids of acquisition, and it is thick to obtain solid-state snake oil Product;
(4) by liquid snake oil crude product described in step (3) and the solid-state snake oil crude product respectively through supercritical CO2Extraction point From step is as follows:It adding in extraction kettle, the extraction temperature of extraction kettle is 38 DEG C, extracting pressure 30Mpa, flow 40L/h, It is then fed into separating still, the pressure of separating still is 22Mpa, and separation temperature is 38 DEG C, and after extracting system stablizes 5min, discharge is dry Initially-separate snake oil in net separating still collects in separating still snake oil to get refined liquid snake oil and refined solid-state snake oil every 1h.
Embodiment 2
(1) the fresh snake oil fat granules of 2kg is taken to be soaked in 6L and contain the vitamin C and mass concentration that mass concentration is 0.05% In pretreatment fluid for 2% sodium chloride, temperature is to stir 5h at 0 DEG C, is repeated 6 times rear drained and standby;
(2) it is the pretreated snake oil fat granule 1kg in step (1) and 10g aluminium oxide, 3kg ether and 0.1g tea is more Phenol is uniformly mixed, and after rotating speed 10000rmp shear agitations 0.5min, after stirring 2h under air-proof condition with rotating speed 200rmp, uses G4 Number sand core funnel filtering, the ether at 30 DEG C in rotary evaporation in vacuo removal filtrate, obtains snake oil crude product;
(3) snake oil in step (2) is added in ether and freezed, the mass ratio of snake oil and ether is 1: 1, -10 DEG C Lower freezing 20h separation of solid and liquid obtains filtrate and solids, and the ether at 30 DEG C in rotary evaporation in vacuo removal filtrate is up to liquid Snake oil crude product mixes the solids with ether, and the mass ratio of solids and ether is 1: 3, is placed in 0 DEG C of environment and freezes 50h, separation of solid and liquid, by the solids of acquisition, rotary evaporation in vacuo removes ether at 30 DEG C, obtains solid-state snake oil crude product;
(4) by liquid snake oil crude product described in step (3) and the solid-state snake oil crude product respectively through supercritical CO2Extraction point From step is as follows:It adding in extraction kettle, the extraction temperature of extraction kettle is 30 DEG C, extracting pressure 45Mpa, flow 20L/h, It is then fed into separating still, the pressure of separating still is 8Mpa, and separation temperature is 40 DEG C, and after extracting system stablizes 5min, discharge is dry Initially-separate snake oil in net separating still collects in separating still snake oil to get refined liquid snake oil and refined solid-state snake oil every 1h.
Embodiment 3
(1) the fresh snake oil fat granules of 2kg is taken to be soaked in 12L and contain the tea polyphenols and mass concentration that mass concentration is 0.03% In pretreatment fluid for 0.1% sodium chloride, temperature is to stir 2h at 25 DEG C, is repeated 2 times rear drained and standby;
(2) by the pretreated snake oil fat granule 1kg in step (1) and 300g silica gel, 10kg ethyl alcohol and 1g vitamin Cs It is uniformly mixed, after rotating speed 200rmp shear agitations 10min, after stirring 0.5h under air-proof condition with rotating speed 1000rmp, with No. G4 Sand core funnel (aperture is 3-4 μm) filters, and the ethyl alcohol at 40 DEG C in rotary evaporation in vacuo removal filtrate obtains snake oil crude product;
(3) snake oil in step (2) is added in ethyl alcohol and freezed, the mass ratio of snake oil and ethyl alcohol is at 1: 3,0 DEG C Freezing 30h separation of solid and liquid obtains filtrate and solids, and the ethyl alcohol at 40 DEG C in rotary evaporation in vacuo removal filtrate is up to liquid snake Oily crude product mixes the solids with ethyl alcohol, and the mass ratio of snake oil and ethyl alcohol is 1: 1, is placed in -5 DEG C of environment and freezes 40h, Separation of solid and liquid, by the solids of acquisition, rotary evaporation in vacuo removes ethyl alcohol at 40 DEG C, obtains solid-state snake oil crude product;
(4) by liquid snake oil crude product described in step (3) and the solid-state snake oil crude product respectively through supercritical CO2Extraction, Step is as follows:It adds in extraction kettle, the extraction temperature of extraction kettle is 40 DEG C, extracting pressure 15Mpa, flow 60L/h, separation The pressure of kettle is 25Mpa, and separation temperature is 30 DEG C, after extracting system stablizes 5min, discharges initially-separate snake in clean separation kettle Oil collects in separating still snake oil to get refined liquid snake oil and refined solid-state snake oil every 1h.
Embodiment 4
A kind of preparation method of snake oil is present embodiments provided, is included the following steps:
(1) take the fresh snake oil fat granules of 15kg be soaked in 45L contain mass concentration be 0.04% citric acid and quality it is dense It spends in the pretreatment fluid for 1.5% sodium chloride, temperature is to impregnate 2h at 10 DEG C, is repeated 5 times rear drained and standby;
(2) by the pretreated snake oil fat granule 1kg in step (1) and 100g activated carbons, 100g atlapulgites, 3kg Acetone, 5kg n-hexanes and 0.8g carnosic acids are uniformly mixed, after rotating speed 6000rmp shear agitations 7min, under air-proof condition with After rotating speed 500rmp stirrings 1.5h, filtered with G4 sand core funnels, acetone at 20 DEG C in rotary evaporation in vacuo removal filtrate and N-hexane obtains snake oil crude product;
(3) snake oil in step (2) is added in the mixed solution of acetone and n-hexane and freezed, snake oil and ethyl alcohol Mass ratio is 1: 2.5, and separation of solid and liquid for 24 hours is freezed at -8 DEG C and obtains filtrate and solids, rotary evaporation in vacuo removes filter at 38 DEG C Acetone and n-hexane in liquid is up to liquid snake oil crude product, and by the solids of acquisition, rotary evaporation in vacuo removes acetone at 38 DEG C Solid-state snake oil crude product is obtained with n-hexane;
(4) by liquid snake oil crude product described in step (3) and the solid-state snake oil crude product respectively through supercritical CO2Extraction, Step is as follows:It adds in extraction kettle, the extraction temperature of extraction kettle is 35 DEG C, extracting pressure 35Mpa, flow 30L/h, then Separating still is sent into, controls the pressure of separating still as 15Mpa, separation temperature is 35 DEG C, and after extracting system stablizes 5min, discharge is clean Initially-separate snake oil in separating still collects in separating still snake oil to get refined liquid snake oil and refined solid-state snake oil every 1h.
Embodiment 5
A kind of snake oil composition is present embodiments provided, including the following raw material:Refined liquid snake oil obtained in embodiment 1 80g, candelila wax 35g, tocopherol 5g and Rosa Damascana 0.3g.
The present embodiment additionally provides the preparation method of above-mentioned snake oil composition, includes the following steps:1) weighed according to formula Raw material;2) candelila wax is heated to melting, stops heating, added in refined liquid snake oil and stir evenly;3) 65 DEG C are cooled to, is added Enter tocopherol and Rosa Damascana, stir evenly;4) 50 DEG C are cooled to, cured bulk is made, cools down to obtain the final product.
Embodiment 6
A kind of snake oil composition is present embodiments provided, including the following raw material:Refined liquid snake oil obtained in embodiment 2 99g and refined solid-state snake oil 1g, tea polyphenols 10g and Lavender 0.01g.
Wherein, the mass percent for refining unrighted acid in liquid snake oil is 70%, refines saturation in solid-state snake oil The mass percent of aliphatic acid is 80%.
The present embodiment additionally provides the preparation method of above-mentioned snake oil composition, includes the following steps:1) weighed according to formula Raw material;2) refined solid-state snake oil is heated to melting, stops heating, added in refined liquid snake oil and stir evenly;3) 70 are cooled to DEG C, tea polyphenols and Lavender are added in, is stirred evenly;4) it is cooled to 55 DEG C, it is filling to be made rodlike, it cools down to obtain the final product.
Embodiment 7
A kind of snake oil composition is present embodiments provided, including the following raw material:Refined liquid snake oil obtained in embodiment 3 40g, refined solid-state snake oil 58g, sesame seed oil 0.01g and Rosemary Oil 0.5g.
Wherein, the mass percent for refining unrighted acid in liquid snake oil is 90%, refines saturation in solid-state snake oil The mass percent of aliphatic acid is 50%.
The present embodiment additionally provides the preparation method of above-mentioned snake oil composition, includes the following steps:1) weighed according to formula Raw material;2) refined solid-state snake oil is heated to melting, stops heating, added in refined liquid snake oil and stir evenly;3) 60 are cooled to DEG C, sesame seed oil and Rosemary Oil are added in, is stirred evenly;4) it is cooled to 52 DEG C, it is filling to be made rodlike, it cools down to obtain the final product.
Embodiment 8
A kind of snake oil composition is present embodiments provided, including the following raw material:Refined liquid snake oil obtained in embodiment 4 60g, hexadecanol 20g, forulic acid 8g, Rosa Damascana 0.3g and Rosemary Oil 0.2g.
Wherein, the mass percent for refining saturated fatty acid in liquid snake oil is 80.3%.
The present embodiment additionally provides the preparation method of above-mentioned snake oil composition, includes the following steps:1) weighed according to formula Raw material;2) hexadecanol is heated to melting, stops heating, added in refined liquid snake oil and stir evenly;3) 62 DEG C are cooled to, is added in Forulic acid, Rosa Damascana and Rosemary Oil, stir evenly;4) it is cooled to 50 DEG C, it is filling to be made rodlike, it cools down to obtain the final product.
Embodiment 9
A kind of snake oil composition is present embodiments provided, including the following raw material:Refined liquid snake oil obtained in embodiment 1 75g, house oil polyunsaturated fatty acid ester 15g, tocopherol 4g, Rosmarinus officinalis extract 2g, Rosa Damascana 0.1g and Lavender 0.05g。
The present embodiment additionally provides the preparation method of above-mentioned snake oil composition, includes the following steps:1) weighed according to formula Raw material;2) refined liquid snake oil and house oil polyunsaturated fatty acid ester are heated to melting, stop heating, added in refined liquid snake oil and stir It mixes uniformly;3) 68 DEG C are cooled to, tocopherol, Rosa Damascana and Lavender is added in, stirs evenly;4) 54 DEG C are cooled to, is filled Cured bulk is made in dress, cools down to obtain the final product.
Comparative example 1
This comparative example provides a kind of preparation method of refined snake oil, includes the following steps:
1) pre-process:Snake fat hair fat 90kg is collected to be refrigerated at 0-4 DEG C, broken obtain meat foam shape little particle;
2) mix:Meat foam shape little particle and rice husk are mixed to get mixture with 1: 4 weight ratio;
3) non-critical fluid extraction:It is extracted normal butane is added in mixture, extracting pressure 6MPa, extraction temperature For 38 DEG C, mixing speed 35rmp;It stands 45min and obtains normal butane extract liquor;
4) vacuum limit takes off normal butane:Collection normal butane extract liquor is transmitted to evaporator and evaporates, the vacuum degree in evaporator For -0.1MPa, 55 DEG C of solution temperature in evaporator, the precipitation time is 50 minutes, evaporates to obtain snake oil primary product;Normal butane is residual Allowance≤300mg/kg;
5) it is transferred to precipitation deodorizing tank:Snake oil primary product are put to transferring in bucket, with transferring, bucket transfer snake oil is primary to be produced Product add in lemon peel into precipitation deodorizing tank, in 3% ratio of solid-liquid weight ratio into precipitation deodorizing tank, and mixing speed is 50rpm, deodorizing time obtain snake oil mixture A when being 4-5 small;Using the heating of chuck hot water in tank, water temperature is 80 DEG C;
6) vacuum takes off normal butane again:Snake oil mixture A is subjected to precipitation deodorizing under conditions of vacuum degree is -0.1MPa Obtain snake oil mixture B;Normal butane residual quantity≤1.0mg/kg after precipitation;Using the heating of chuck hot water, water temperature 80 in tank ℃;
7) separation of solid and liquid:Refined snake oil is obtained by filtration in snake oil mixture B, and transmission snake oil is in collecting vessel;Metering, sealing, patch Label;Loaded on container.
The present embodiment additionally provides a kind of snake oil composition, the snake oil composition and preparation method and 5 base of embodiment This is identical, differs only in refined snake oil therein and is substituted for refined snake oil manufactured in the present embodiment.
Experimental example 1
Pretreated fresh snake oil fat granule and the fresh snake oil fat without pretreatment in 100g embodiments 1 are weighed respectively Grain is separately added into 300g n-hexanes respectively as in 500ml beakers, with rotating speed 5000rmp shear agitations 3min to without apparent Adipose tissue stirs 1h under air-proof condition with rotating speed 800rmp, and transparence snake oil is respectively obtained by the filtering of G4 sand core funnels Hexane solution, by removing n-hexane at 35 DEG C of vacuum rotary evaporator, be respectively compared pretreated snake oil with without pre- place The color and fishy smell of the snake oil of reason, concrete outcome are shown in Table 1.
1 pretreating effect of table compares
Pre-process snake oil Without pretreatment snake oil
Color It is golden yellow Buff
Fishy smell Gently Weight
As it can be seen from table 1 the snake oil fat granule of pretreatment, color is more of light color than the snake oil of no pretreatment, and fishy smell is small, Snake oil part colours and fishy smell are can remove by pre-processing.
Experimental example 2
Pretreated snake fat in 100g embodiments 1 is weighed respectively, as in 1000ml beakers, is separately added into 0.1g lemons Lemon acid, atlapulgite, silica gel, aluminium oxide or the activated carbon of 600g n-hexanes and 5g, with rotating speed 5000rmp shear agitation 2min, 1h is stirred with rotating speed 500rmp under air-proof condition, it is molten to respectively obtain transparence snake oil n-hexane by the filtering of G4 sand core funnels Liquid finally by n-hexane is removed at 35 DEG C of vacuum rotary evaporator, measures snake oil quality, color and smell situation, tool respectively Body is shown in Table 2.
2 adsorbent effect of table compares
Adsorbent Quality/g Color Fishy smell
Without adsorbent 78 It is golden yellow Weight
Atlapulgite 67 It is light yellow It is light
Silica gel 67 It is light yellow It is light
Neutral alumina 66 It is light yellow It is light
Activated carbon 63 It is light yellow It is thin
From table 2 it can be seen that addition adsorbent effectively can carry out decoloration deodorization to snake oil.
Experimental example 3
Weigh and snake fat pre-processed in 100g embodiments 1 as in 2000ml beakers, add in 0.1g citric acids, 800g just oneself Alkane and 5g atlapulgites, with rotating speed 5000rmp shear agitation 2min, are stirred 1h with rotating speed 800rmp, passed through by high speed shear Transparence snake oil hexane solution is obtained by filtration in G4 sand core funnels, by removing n-hexane at 35 DEG C of vacuum rotary evaporator, Obtain the snake oil that atlapulgite is first handled.
Snake fat pretreated in 100g embodiments 1 is weighed as in 2000ml beakers, adds in 0.1g citric acids, 800g With rotating speed 5000rmp shear agitation 2min, transparence snake oil n-hexane is respectively obtained by the filtering of G4 sand core funnels for n-hexane Solution by removing n-hexane at 35 DEG C of vacuum rotary evaporator, then adds in 5g atlapulgites, with rotating speed into snake oil 800rmp stirs 1h, and centrifugation obtains the snake oil of atlapulgite post processing, compares the color and smell of above-mentioned two groups of snake oils, specific to tie Fruit is shown in Table 4.
3 adsorbent of table adds and adding order compares
Adsorbent Color Fishy smell
Without adsorbent It is golden yellow Weight
First add in atlapulgite It is light yellow It is light
After add in atlapulgite It is golden yellow Weight
As can be seen from Table 3, atlapulgite ratio is added in snake oil hexane solution, atlapulgite tool is added in pure snake oil There is the effect that more effectively decoloration is deodorized.
Experimental example 4
Under room temperature, snake fat pretreated in 100g embodiments 1 is weighed respectively as in 500ml beakers, is distinguished The atlapulgite of 0.1g citric acids, 300g n-hexanes and 1g, 2.5g, 5g, 10g, 20g and 30g are added in, is cut with rotating speed 10000rmp Stirring 2min is cut, after stirring 30min under air-proof condition with rotating speed 800rmp, is respectively obtained by the filtering of G4 sand core funnels transparent Shape snake oil hexane solution, by removing n-hexane at 35 DEG C of vacuum rotary evaporator, relatively the quality of gained snake oil, color and Smell is specifically shown in Table 4.
4 adsorbent additive amount effect of table compares
Atlapulgite additive amount/g Snake oil quality g Color Fishy smell
1 77 ***** *****
2.5 75 **** ****
5 72 *** ***
10 67 ** **
20 65 * *
30 58 * *
Note:* bright color of more saving your breath is lighter or fishy smell is lighter.
As can be seen from Table 4, more with the additive amount of atlapulgite, the color of snake oil is lighter, and fishy smell is also got over Light, addition atlapulgite can reduce the fishy smell of snake oil.
Experimental example 5
Refined liquid snake oil obtained is consolidated with refined during subject is to embodiment 1 under room temperature (25 DEG C), high temperature (40 DEG C) The smell of snake oil obtained is given a mark (5 points of systems) in state snake oil and comparative example 1, and the more heavy then score value of smell is higher, the experimenter Group is 30 people, and point value of evaluation is arithmetic mean of instantaneous value, is specifically shown in Table 1.
5 smell of table compares
As can be seen from Table 5, subject is for refined liquid snake oil obtained and refined solid-state snake oil acceptance in embodiment 1 Height, snake oil preparation method provided by the invention can effectively remove the fishy smell of snake oil.
Experimental example 6
Constituent analysis is carried out to refined liquid snake oil obtained in embodiment 1 and refined solid-state snake oil, is specifically shown in Table 6.
6 snake oil constituent analysis of table
As can be seen from Table 6, total unsaturated fatty acid content of refined liquid snake oil obtained is 75.3% in embodiment 1, Total saturated fatty acid content of refined solid-state snake oil is 59.4%.
Experimental example 7
Peroxide value and acid value determination, tool are carried out to the refined liquid snake oil obtained in embodiment 1 and refined solid-state snake oil Body the results are shown in Table 7.
7 peroxide value of table and acid value determination
Sample Refined liquid snake oil Refined solid-state snake oil
Fusing point (DEG C) Room temperature is liquid 55
Color It is faint yellow White
Peroxide value meq/kg 1.02 1.26
Acid value mL/L 0.41 0.33
As can be seen from Table 7, in embodiment 1 peroxide value of refined liquid snake oil obtained and refined solid-state snake oil and Acid value is low, and the stability of snake oil is good.
Experimental example 8
Snake oil composition made from embodiment 5, comparative example 1 is tested for the property:Experimenter's skin health, forearm are different Different disposal is done in region, with Courage+Khazaka Multi Skin Test Center MC750 test different disposals region Skin moisture content, take mathematical mean, be specifically shown in Table 8.
It is untreated:Normal skin does not smear any product;
Damaged skin:With adhesive sticker skin surface paste, tear, be repeated 3 times;
Test skin:Impaired treated dermal application snake oil stick, 0.01g/cm2
8 moisture content of skin of table is tested
As can be seen from Table 8, snake oil composition obtained is mended compared with the snake oil composition of comparative example 1 in embodiment 5 Water effect is more preferable, has maintenance effect for damaged skin.
Obviously, the above embodiments are merely examples for clarifying the description, and is not intended to limit the embodiments.It is right For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or It changes.There is no necessity and possibility to exhaust all the enbodiments.And the obvious variation thus extended out or Among changing still in the protection domain of the invention.

Claims (10)

1. a kind of snake oil composition, which is characterized in that including the following raw material:Refined snake oil 40-99 parts by weight, assistant formation agent 1- 58 parts by weight, antioxidant 0.01-10 parts by weight and plants essential oil 0.01-0.5 parts by weight.
2. snake oil composition according to claim 1, which is characterized in that including the following raw material:80 parts by weight of refined snake oil, 0.3 parts by weight of 35 parts by weight of assistant formation agent, 5 parts by weight of antioxidant and plants essential oil.
3. snake oil composition according to claim 1 or 2, which is characterized in that the refined snake oil is refined liquid snake Oil;Preferably, the mass percent of unrighted acid is 70-90% in the liquid snake oil.
4. according to the snake oil composition described in claim 1-3 any one, which is characterized in that the assistant formation agent is snake oil Saturated fatty acid, the saturated fatty alcohol in other animal or plant sources, one or more of mixtures of polyunsaturated fatty acid ester or wax.
5. according to the snake oil composition described in claim 1-4 any one, which is characterized in that the preparation side of the refined snake oil Method includes the following steps:
(1) snake oil fat granule is taken to be pre-processed;
(2) snake oil fat granule pretreated in step (1) is added in low boiling point organic solvent, while adds in adsorbent and resist Oxidant, under room temperature shear agitation, filtering, removes the low boiling point organic solvent in gained filtrate, obtains snake oil;
(3) snake oil into step (2) is added in low boiling point organic solvent and freezed, and separation of solid and liquid obtains filtrate and solid Object, removal low boiling point organic solvent obtain liquid snake oil crude product and solid-state snake oil crude product;
(4) the liquid snake oil crude product and solid-state snake oil crude product that are obtained in step (3) are subjected to decoloration deodorization respectively.
6. snake oil composition according to claim 5, which is characterized in that in the step (2), the low boiling point is organic Solvent is at least one of n-hexane, ether, ethyl alcohol or acetone;The adsorbent is atlapulgite, aluminium oxide, silica gel or work At least one of property charcoal;The antioxidant is at least one of citric acid, vitamin C or tea polyphenols;Preferably, it is described Low boiling point organic solvent is n-hexane;Preferably, the adsorbent is atlapulgite.
7. according to the snake oil composition described in claim 1-6 any one, which is characterized in that the antioxidant is fertility At least one of phenol, sesame seed oil, forulic acid, tea polyphenols or Rosmarinus officinalis extract.
8. according to the snake oil composition described in claim 1-7 any one, which is characterized in that the plants essential oil is rhodamine toner At least one of oil, Lavender or Rosemary Oil.
A kind of 9. method for preparing the snake oil composition as described in claim 1-8 any one, which is characterized in that including as follows Step:
1) raw material is weighed according to formula;
2) assistant formation agent is heated to melting, stops heating, added in the refined snake oil and stir evenly;
3) 60-70 DEG C is cooled to, the antioxidant and the plants essential oil is added in, stirs evenly;
4) 50-55 DEG C is cooled to, filling, cooling.
10. snake oil combination prepared by the method described in the snake oil composition or claim 9 described in claim 1-8 any one Purposes of the object in terms of drug or daily chemical product is prepared.
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