CN107496269A - A kind of cinnamon bark extract and preparation method thereof and the application in cosmetics - Google Patents

A kind of cinnamon bark extract and preparation method thereof and the application in cosmetics Download PDF

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CN107496269A
CN107496269A CN201710970697.9A CN201710970697A CN107496269A CN 107496269 A CN107496269 A CN 107496269A CN 201710970697 A CN201710970697 A CN 201710970697A CN 107496269 A CN107496269 A CN 107496269A
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cinnamon bark
extract
cinnamon
preparation
powder
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冼嘉星
裴运林
聂艳峰
刘露
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Guangdong Marubi Biological Technology Co Ltd
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Guangdong Marubi Biological Technology 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
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/02Preparations for care of the skin for chemically bleaching or whitening the skin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/08Anti-ageing preparations
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/74Biological properties of particular ingredients
    • A61K2800/75Anti-irritant
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/74Biological properties of particular ingredients
    • A61K2800/78Enzyme modulators, e.g. Enzyme agonists
    • A61K2800/782Enzyme inhibitors; Enzyme antagonists
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/805Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/82Preparation or application process involves sonication or ultrasonication

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  • Cosmetics (AREA)

Abstract

The invention belongs to the technical field of cosmetics, discloses a kind of cinnamon bark extract and preparation method thereof and the application in cosmetics.Methods described is:(1) ungrease treatment is carried out to cinnamon bark powder using solvent, filtering, filter residue is dried, obtains degreasing cinnamon bark powder;(3) ethanol water is mixed with degreasing cinnamon bark powder, ultrasonic extraction, filtered, filtrate stands, and takes subnatant, is concentrated under reduced pressure, frozen dried, obtains powdered cinnamon bark crude extract;(5) volume fraction is used to be dissolved cinnamon bark crude extract for 5%~15% ethanol water, purified again using macroreticular resin gel column, eluted, be concentrated under reduced pressure for 30%~90% ethanol water with volume fraction, it is lyophilized, obtain cinnamon bark extract after purification.The cinnamon bark extract recovery rate of the present invention is high, and inoxidizability and whitening effect are good, are made antidotal agent or whitening agent is applied in cosmetics.

Description

A kind of cinnamon bark extract and preparation method thereof and the application in cosmetics
Technical field
The invention belongs to the technical field of cosmetics, is related to a kind of cinnamon bark extract, and in particular to one kind contains Huang Cinnamon bark extract of ketone and tannic acid and preparation method thereof and the application in cosmetics.
Background technology
Chinese cassia tree (Classification system:Cinnamomum cassia Presl), also known as beautiful osmanthus, male osmanthus, cajaput, great Gui, peppery osmanthus, Safety tree, cassia, it is the dry bark of canella Chinese cassia tree.It is a kind of conventional food because cinnamon bark fragrant odour It is deep to be liked by masses with spices.In addition, as the ancient country with succession in more than 5,000 years, the medical value of cinnamon bark It is early on the books,《Chinese Pharmacopoeia》In, the primary efficacy for recording cinnamon bark is mends fire supporing yang, let the fire back to its origin, eliminating cold to stop pain, is lived Blood stimulates the menstrual flow.For impotence, Gong Leng, waist and knee crymodynia, deficiency of the kidney and dyspnea, dizziness due to yang deficiency, hot eyes pharyngalgia, trusted subordinate's crymodynia, cold of insufficiency type vomiting and diarrhea, tremble with fear Hernia, run quickly globefish, Amenorrhea, dysmenorrhoea.
Application and development for cinnamon bark, in the market are mostly that cinnamon oil is extracted from cinnamon bark, however, cinnamon oil Content accounts for the 1.98-2.06% of cinnamon bark, and wherein cinnamic acid accounts for 53%-61%, is intended only as aromatic use.Meat Also contain many other compositions in cassia tree skin.
Extract functional component from plant, in general method has a water-boiling method, solvent method, the methods of super critical extraction.So And the extraction time that water-boiling method needs is longer, production efficiency is more low.Solvent method needs to use some such as carbon dichloride etc. Organic solvent, easily residual is in the sample, obviously improper as cosmetic industry raw material for organic solvent.Super critical extraction is A kind of extracting method compared with high technology content, but production cost is higher.
The present invention uses ultrasonic extraction, not only increases the recovery rate of cinnamon bark extract, moreover it is possible to greatly shorten and carry The time is taken, compared with low production cost, is adapted to large-scale production.The present invention is by ultrasonic extraction, by macroporous resin purification, and will be pure Extract after change is applied in cosmetics, can meet multiple efficacies demand of the consumer to cosmetics, very with market Prospect.The cinnamon bark extract of the present invention has extraordinary anti-oxidant and whitening effect.
The content of the invention
In order to overcome in the prior art extract recovery rate it is not high, improve the purity of extract, obtain high content xylocinnamomum Skin active ingredient, it is an object of the invention to provide a kind of cinnamon bark extract and preparation method thereof.The present invention passes through ultrasound Active ingredient in assisted extraction cinnamon bark, improve the recovery rate of extract;, can be by xylocinnamomum by the way that crude extract is purified Bark extract is applied directly in cosmetics.Flavones and tannic acid kind compound content in the cinnamon bark extract of the present invention Height, there is extraordinary anti-oxidant and whitening effect.
Another object of the present invention is to provide the application of above-mentioned cinnamon bark extract.The cinnamon bark extract is used In the cosmetics for preparing anti-aging and/or whitening.
The purpose of the present invention is achieved through the following technical solutions:
A kind of preparation method of cinnamon bark extract, comprises the following steps:
(1) cinnamon bark is crushed, sieved, drying, obtain cinnamon bark powder;
(2) ungrease treatment is carried out to cinnamon bark powder using solvent, filtering, filter residue is dried, obtains degreasing xylocinnamomum Skin powder;
(3) ethanol water is mixed with degreasing cinnamon bark powder, the ultrasonic extraction under conditions of 30~70 DEG C, mistake Filter, filtrate stratification, removes a layer stillness of night, obtains cinnamon bark crude extract;
(4) cinnamon bark crude extract is concentrated under reduced pressure, frozen dried, obtains powdered cinnamon bark crude extract;
(5) use volume fraction to be dissolved cinnamon bark crude extract for 5%~15% ethanol water, then use Macroreticular resin gel column purifies, and is that eluent is eluted using volume fraction as 30%~90% ethanol water, will elute Thing is concentrated under reduced pressure, and is freezed, is obtained cinnamon bark extract after purification.
The temperature dried described in step (1) is 40~50 DEG C;It is petroleum ether, ether or second to hold agent described in step (2) Acetoacetic ester, the mass ratio of the cinnamon bark powder and solvent is 1:(10~100);The condition of the ungrease treatment is under normal temperature 0.5-5h is stirred, the temperature of the drying is 40~50 DEG C;Described in step (3) in ethanol water ethanol percentage by volume For 0~80%, preferably 40%~80%;The mass volume ratio of degreasing cinnamon bark powder and ethanol water for (1.0~ 6.0)g:120mL, preferably 1g:(40~80) mL;The power of ultrasonic extraction is 0~800W, preferably 400~800W;Ultrasound The time of extraction is 0.25~2.5h;The temperature of the extraction is preferably 40 DEG C~60 DEG C;
Eluent described in step (5) is preferably that volume fraction is 75% ethanol water;
The potting resin of macroreticular resin gel column described in step (5) be D101, D4020, HPD-100, DM130, AB-8, One kind in S-8, ADS-17, DA-201C, HPD-400 and MAK- II, but it is not limited only to this.
The volume ratio of volume and gel column after the dissolving of cinnamon bark crude extract described in step (5) is 1:15~1:40; Preferably 1:25, so more preferably active ingredient can be separated with impurity faster.
The ratio between the post footpath of macroreticular resin gel column and pillar height are essentially that higher separating effect is better, but in the present invention such as Fruit ratio exceeds 1:85 flow velocitys are excessively slow, influence the efficiency of separation and Extraction, and when the ratio between post footpath and pillar height are less than 1:Then can when 40 Cause that impurity can not be sufficiently separated;Therefore, the ratio between the post footpath of macroreticular resin gel column and pillar height are 1:40~1:85, preferably 1: 50。
When being purified using macroreticular resin gel column, loading flow velocity is 1.0~6.0ml/min.
The condition being concentrated under reduced pressure described in step (5) is:Temperature is 40~50 DEG C, and rotary speed is 100~120rpm.
Active constituent content determines by the following method in the cinnamon bark crude extract:
Respectively using rutin and tannic acid as standard items, establish measure using ultraviolet specrophotometer and extracted from cinnamon bark The standard curve of flavones and tannic acid;Using ultraviolet specrophotometer and standard curve, determine yellow in cinnamon bark crude extract The content of ketone and tannic acid.
The cinnamon bark extract is prepared by the above method.
The cinnamon bark extract is used for the cosmetics for preparing anti-aging and/or whitening.
In cinnamon bark crude extract, containing more impurity, electrical conductivity is higher, can be to making up when being applied in cosmetics The emulsification system of product causes serious destruction, therefore, it is necessary to carries out purification process to cinnamon bark crude extract.In order to obtain more Pure cinnamon bark extract, cinnamon bark flavones and tannic acid crude extract are purified from macroreticular resin gel column, can be with The impurity in crude extract is removed to greatest extent, and is enriched with the content of flavones and tannic acid.
Contain abundant flavones and tannin acid, the recovery rate of extract in the cinnamon bark extract of the present invention Height, when the extract is used in cosmetics, flavones and tannin acid cooperate so that cinnamon bark extract has There are extraordinary inoxidizability and whitening effect.The extract of the present invention can effectively remove the oxygen radical in human body, prevent The degeneration and aging of cell, while inflammatory biology enzyme can also be suppressed, wound healing and analgesic can be promoted, can be with anti-inflammatory and anti-mistake It is quick;And stronger convergence effect can also be played, suppresses the activity of tyrosinase, removes free radical, moisture of skin is kept, has Antisepsis.
Compared with prior art, the present invention has advantages below and beneficial effect:
(1) cinnamon bark extract of the invention has extraordinary inoxidizability and whitening effect, is made anti-aging Agent or whitening agent are applied in cosmetics, have fabulous effect;
(2) present invention utilizes the flavones and tannin acid in ultrasound assisted extraction cinnamon bark, and extraction time relatively passes System extracting method substantially reduces, and extraction efficiency is high, and the extracted amount of tannic acid is 41.9~91.3mg/g in crude extract, yellow The extracted amount of ketone is 103.6~172.1mg/g;Tannin acid content reaches 31.11% (matter in cinnamon bark extract after purification Measure fraction), 49.04% is improved than cinnamon bark crude extract tannin acid content, flavones content after purification reaches 93.62% (mass fraction), improves 64.21%;
(3) macroreticular resin selected of the present invention, have to the flavones in cinnamon bark and tannic acid high adsorption efficiency and Desorption efficiency, the tannic acid and flavones content of obtained extract are high.
Embodiment
Further detailed description is done to the present invention with reference to specific embodiment, but embodiments of the present invention are not limited to This.The method that standard curve used is established in following embodiments unless otherwise specified, is conventional method, made in embodiment Raw material, reagent etc., unless otherwise specified, being can be from the raw material and reagent that routinely the commercial sources such as purchased in market obtain.
It is the method that standard curve is established below:
(1) standard curve for determining cinnamon bark extract tannin acid content is established
1. the fresh sodium carbonate liquor for preparing 75g/L:
2. the fresh tannin standard acid solution for preparing 0.1mg/ml:
3. respectively toward accurately add in 6 10ml volumetric flasks freshly prepared tannin standard acid solution 0,0.2,0.4,0.5, 0.6th, 0.8ml, then toward addition 0.8ml Folin-Denis developers in volumetric flask, shake up, stand 5min, add 2.0ml's 75g/L sodium carbonate liquor, shakes up, and stands 5min, then is settled to graduation mark with distilled water, shakes up, and stands 30min, then with dividing Light photometer measurement absorbance is the light absorption value at 752nm, establishes standard curve, standard curve is:
Y=94.5X+0.048R2=0.999 wherein, and Y value is light absorption value, and X is the concentration of tannic acid in volumetric flask, unit For mg/ml;R is linearly dependent coefficient;
(2) standard curve for determining cinnamon bark extract flavones content is established
1. the fresh sodium nitrite solution for preparing 5g/100ml;
2. the fresh liquor alumini chloridi for preparing 10g/100ml;
3. the fresh sodium hydroxide solution for preparing 1mol/L;
4. take 0.06,0.08,0.12,0.16,0.20mg/ml standard liquid 2ml be placed in test tube, add 0.2ml's 5g/100ml sodium nitrite solution, shakes up, and stands 6min, adds 0.2ml 10g/100ml liquor alumini chloridi 0.2ml, Shake up, stand 6min, add 2ml 1mol/L sodium hydroxide solution, shake up, stand 30min, then measured with spectrophotometric It is the light absorption value at 510nm to measure absorbance, establishes standard curve, standard curve is:
Y=1.650X-0.017R2=0.999 wherein, and Y is light absorption value, and X is flavones total amount, unit mg.
In embodiment 1~7 and comparative example 2, when being purified, the ratio between the post footpath of macroreticular resin gel column and pillar height are 1:50, the volume ratio of volume and gel column after the cinnamon bark crude extract dissolving is 1:25, so can be more preferably faster Active ingredient is separated with impurity.When being purified using macroreticular resin gel column, flow velocity 3.0ml/min.It is big using D101 Hole resin gel post is purified.
Embodiment 1
A kind of preparation method of cinnamon bark extract, comprises the following steps:
(1) cinnamon bark is crushed using medicinal herb grinder, crosses 60 mesh sieves, be dried to constant weight in 45 DEG C, obtain xylocinnamomum Skin powder;
(2) (cinnamon bark powder is mixed to cinnamon bark powder using ether:The mass ratio of ether is 1:60), stir 1h, filtering, is dried to constant weight in 45 DEG C by filter residue, obtains degreasing cinnamon bark powder;Weight is recovered by distillation in ether in filtrate It is multiple to utilize;
(3) in a reservoir, the ethanol water and 3.0g degreasing cinnamon bark powder for being 40% by 120mL percentage by volumes Mixing, sealing, with 400W ultrasonic power ultrasonic extraction 1h under conditions of 40 DEG C, filtering, filtrate stratification, it is clear to remove layer At night, obtain cinnamon bark crude extract;The content of tannic acid is 75.5mg/g (i.e. each gram of Chinese cassia trees in cinnamon bark crude extract Bark fines can extract 75.45mg tannic acid), the content of flavones is 136.8mg/g;
(4) cinnamon bark crude extract being concentrated under reduced pressure, (- 0.1MPa vacuum, rotary speed 115rpm/min, evaporation are warm 45 DEG C of degree, 2 DEG C of circulating condensing temperature), frozen dried (- 78 DEG C of cryogenic temperature, cooling time 48h, vacuum pressure 20Pa), obtain powder Last shape cinnamon bark crude extract;
(5) use volume fraction that powdered cinnamon bark crude extract is dissolved into (ethanol for 10% ethanol water The aqueous solution and the amount ratio of cinnamon bark crude extract are 100mL:1g), obtain redissolving liquid;Liquid will be redissolved and use D101 macropore trees Fat gel column purifies, and is that eluent is eluted using volume fraction as 75% ethanol water, eluate depressurize dense Contract (- 0.1MPa vacuum, rotary speed 115rpm/min, 45 DEG C of evaporating temperature, 2 DEG C of circulating condensing temperature), frozen dried is (cold Freeze -78 DEG C of temperature, cooling time 48h, vacuum pressure 20Pa), obtain cinnamon bark extract after purification.Purified in the present embodiment The weight/mass percentage composition of tannic acid is 18.74% in cinnamon bark extract afterwards, and the weight/mass percentage composition of flavones is 79.26%.
Embodiment 2
A kind of preparation method of cinnamon bark extract, comprises the following steps:
(1) cinnamon bark is crushed using medicinal herb grinder, crosses 60 mesh sieves, be dried to constant weight in 45 DEG C, obtain xylocinnamomum Skin powder;
(2) (cinnamon bark powder is mixed to cinnamon bark powder using ether:The mass ratio of ether is 1:60), stir 1h, filtering, is dried to constant weight in 45 DEG C by filter residue, obtains degreasing cinnamon bark powder;Weight is recovered by distillation in ether in filtrate It is multiple to utilize;
(3) in a reservoir, the ethanol water and 1.5g degreasing cinnamon bark powder for being 40% by 120mL percentage by volumes Mixing, sealing, with 720W ultrasonic power ultrasonic extraction 2h under conditions of 60 DEG C, filtering, filtrate stratification, it is clear to remove layer At night, obtain cinnamon bark crude extract;The content of tannic acid is 87.5mg/g in cinnamon bark crude extract, and the content of flavones is 168.0mg/g;
(4) cinnamon bark crude extract being concentrated under reduced pressure, (- 0.1MPa vacuum, rotary speed 115rpm/min, evaporation are warm 45 DEG C of degree, 2 DEG C of circulating condensing temperature), frozen dried (- 78 DEG C of cryogenic temperature, cooling time 48h, vacuum pressure 20Pa), obtain powder Last shape cinnamon bark crude extract;
(5) use volume fraction that powdered cinnamon bark crude extract is dissolved into (ethanol for 10% ethanol water The aqueous solution and the amount ratio of cinnamon bark crude extract are 100mL:1g), obtain redissolving liquid;Liquid will be redissolved and use D101 macropore trees Fat gel column purifies, and is that eluent is eluted using volume fraction as 75% ethanol water, eluate depressurize dense Contract (- 0.1MPa vacuum, rotary speed 115rpm/min, 45 DEG C of evaporating temperature, 2 DEG C of circulating condensing temperature), frozen dried is (cold Freeze -78 DEG C of temperature, cooling time 48h, vacuum pressure 20Pa), obtain cinnamon bark extract after purification.Purified in the present embodiment The weight/mass percentage composition of tannic acid is 29.07% in cinnamon bark extract afterwards, and the weight/mass percentage composition of flavones is 90.83%.
Embodiment 3
A kind of preparation method of cinnamon bark extract, comprises the following steps:
(1) cinnamon bark is crushed using medicinal herb grinder, crosses 60 mesh sieves, be dried to constant weight in 45 DEG C, obtain xylocinnamomum Skin powder;
(2) (cinnamon bark powder is mixed to cinnamon bark powder using ether:The mass ratio of ether is 1:60), stir 1h, filtering, is dried to constant weight in 45 DEG C by filter residue, obtains degreasing cinnamon bark powder;Weight is recovered by distillation in ether in filtrate It is multiple to utilize;
(3) in a reservoir, the ethanol water and 1.5g degreasing cinnamon bark powder for being 60% by 120mL percentage by volumes Mixing, sealing, with 400W ultrasonic power ultrasonic extraction 1h under conditions of 60 DEG C, filtering, filtrate stratification, it is clear to remove layer At night, obtain cinnamon bark crude extract;The content of tannic acid is 88.5mg/g in cinnamon bark crude extract, and the content of flavones is 166.6mg/g;
(4) cinnamon bark crude extract being concentrated under reduced pressure, (- 0.1MPa vacuum, rotary speed 115rpm/min, evaporation are warm 45 DEG C of degree, 2 DEG C of circulating condensing temperature), frozen dried (- 78 DEG C of cryogenic temperature, cooling time 48h, vacuum pressure 20Pa), obtain powder Last shape cinnamon bark crude extract;
(5) use volume fraction that powdered cinnamon bark crude extract is dissolved into (ethanol for 10% ethanol water The aqueous solution and the amount ratio of cinnamon bark crude extract are 100mL:1g), obtain redissolving liquid;Liquid will be redissolved and use D101 macropore trees Fat gel column purifies, and is that eluent is eluted using volume fraction as 75% ethanol water, eluate depressurize dense Contract (- 0.1MPa vacuum, rotary speed 115rpm/min, 45 DEG C of evaporating temperature, 2 DEG C of circulating condensing temperature), frozen dried is (cold Freeze -78 DEG C of temperature, cooling time 48h, vacuum pressure 20Pa), obtain cinnamon bark extract after purification.Purified in the present embodiment The weight/mass percentage composition of tannic acid is 29.32% in cinnamon bark extract afterwards, and the weight/mass percentage composition of flavones is 90.48%.
Embodiment 4
A kind of preparation method of cinnamon bark extract, comprises the following steps:
(1) cinnamon bark is crushed using medicinal herb grinder, crosses 60 mesh sieves, be dried to constant weight in 45 DEG C, obtain xylocinnamomum Skin powder;
(2) (cinnamon bark powder is mixed to cinnamon bark powder using ether:The mass ratio of ether is 1:60), stir 1h, filtering, is dried to constant weight in 45 DEG C by filter residue, obtains degreasing cinnamon bark powder;Weight is recovered by distillation in ether in filtrate It is multiple to utilize;
(3) in a reservoir, the ethanol water and 1.5g degreasing cinnamon bark powder for being 80% by 120mL percentage by volumes Mixing, sealing, with 560W ultrasonic power ultrasonic extraction 2h under conditions of 40 DEG C, filtering, filtrate stratification, it is clear to remove layer At night, obtain cinnamon bark crude extract;The content of tannic acid is 73.0mg/g in cinnamon bark crude extract, and the content of flavones is 139.1mg/g;
(4) cinnamon bark crude extract being concentrated under reduced pressure, (- 0.1MPa vacuum, rotary speed 115rpm/min, evaporation are warm 45 DEG C of degree, 2 DEG C of circulating condensing temperature), frozen dried (- 78 DEG C of cryogenic temperature, cooling time 48h, vacuum pressure 20Pa), obtain powder Last shape cinnamon bark crude extract;
(5) use volume fraction that powdered cinnamon bark crude extract is dissolved into (ethanol for 10% ethanol water The aqueous solution and the amount ratio of cinnamon bark crude extract are 100mL:1g), obtain redissolving liquid;Liquid will be redissolved and use D101 macropore trees Fat gel column purifies, and is that eluent is eluted using volume fraction as 75% ethanol water, eluate depressurize dense Contract (- 0.1MPa vacuum, rotary speed 115rpm/min, 45 DEG C of evaporating temperature, 2 DEG C of circulating condensing temperature), frozen dried is (cold Freeze -78 DEG C of temperature, cooling time 48h, vacuum pressure 20Pa), obtain cinnamon bark extract after purification.Purified in the present embodiment The weight/mass percentage composition of tannic acid is 17.63% in cinnamon bark extract afterwards, and the weight/mass percentage composition of flavones is 79.88%.
Embodiment 5
A kind of preparation method of cinnamon bark extract, comprises the following steps:
(1) cinnamon bark is crushed using medicinal herb grinder, crosses 60 mesh sieves, be dried to constant weight in 45 DEG C, obtain xylocinnamomum Skin powder;
(2) (cinnamon bark powder is mixed to cinnamon bark powder using ether:The mass ratio of ether is 1:60), stir 1h, filtering, is dried to constant weight in 45 DEG C by filter residue, obtains degreasing cinnamon bark powder;Weight is recovered by distillation in ether in filtrate It is multiple to utilize;
(3) in a reservoir, the ethanol water and 1.5g degreasing cinnamon bark powder for being 40% by 120mL percentage by volumes Mixing, sealing, with 400W ultrasonic power ultrasonic extraction 1.5h under conditions of 50 DEG C, filtering, filtrate stratification, it is clear to remove layer At night, obtain cinnamon bark crude extract;The content of tannic acid is 87.7mg/g in cinnamon bark crude extract, and the content of flavones is 164.5mg/g;
(4) cinnamon bark crude extract being concentrated under reduced pressure, (- 0.1MPa vacuum, rotary speed 115rpm/min, evaporation are warm 45 DEG C of degree, 2 DEG C of circulating condensing temperature), frozen dried (- 78 DEG C of cryogenic temperature, cooling time 48h, vacuum pressure 20Pa), obtain powder Last shape cinnamon bark crude extract;
(5) use volume fraction that powdered cinnamon bark crude extract is dissolved into (ethanol for 10% ethanol water The aqueous solution and the amount ratio of cinnamon bark crude extract are 100mL:1g), obtain redissolving liquid;Liquid will be redissolved and use D101 macropore trees Fat gel column purifies, and is that eluent is eluted using volume fraction as 75% ethanol water, eluate depressurize dense Contract (- 0.1MPa vacuum, rotary speed 115rpm/min, 45 DEG C of evaporating temperature, 2 DEG C of circulating condensing temperature), frozen dried is (cold Freeze -78 DEG C of temperature, cooling time 48h, vacuum pressure 20Pa), obtain cinnamon bark extract after purification.Purified in the present embodiment The weight/mass percentage composition of tannic acid is 28.55% in cinnamon bark extract afterwards, and the weight/mass percentage composition of flavones is 89.62%.
Embodiment 6
A kind of preparation method of cinnamon bark extract, comprises the following steps:
(1) cinnamon bark is crushed using medicinal herb grinder, crosses 60 mesh sieves, be dried to constant weight in 45 DEG C, obtain xylocinnamomum Skin powder;
(2) (cinnamon bark powder is mixed to cinnamon bark powder using ether:The mass ratio of ether is 1:60), stir 1h, filtering, is dried to constant weight in 45 DEG C by filter residue, obtains degreasing cinnamon bark powder;Weight is recovered by distillation in ether in filtrate It is multiple to utilize;
(3) in a reservoir, the ethanol water that 120mL percentage by volumes are 80% is mixed with 2g degreasing cinnamon bark powder Close, sealing, with 400W ultrasonic power ultrasonic extraction 2h under conditions of 40 DEG C, filtering, filtrate stratification, remove a layer stillness of night, Obtain cinnamon bark crude extract;The content of tannic acid is 68.3mg/g in cinnamon bark crude extract, and the content of flavones is 125.1mg/g;
(4) cinnamon bark crude extract being concentrated under reduced pressure, (- 0.1MPa vacuum, rotary speed 115rpm/min, evaporation are warm 45 DEG C of degree, 2 DEG C of circulating condensing temperature), frozen dried (- 78 DEG C of cryogenic temperature, cooling time 48h, vacuum pressure 20Pa), obtain powder Last shape cinnamon bark crude extract;
(5) use volume fraction that powdered cinnamon bark crude extract is dissolved into (ethanol for 10% ethanol water The aqueous solution and the amount ratio of cinnamon bark crude extract are 100mL:1g), obtain redissolving liquid;Liquid will be redissolved and use D101 macropore trees Fat gel column purifies, and is that eluent is eluted using volume fraction as 75% ethanol water, eluate depressurize dense Contract (- 0.1MPa vacuum, rotary speed 115rpm/min, 45 DEG C of evaporating temperature, 2 DEG C of circulating condensing temperature), frozen dried is (cold Freeze -78 DEG C of temperature, cooling time 48h, vacuum pressure 20Pa), obtain cinnamon bark extract after purification.Purified in the present embodiment The weight/mass percentage composition of tannic acid is 15.71% in cinnamon bark extract afterwards, and the weight/mass percentage composition of flavones is 70.93%.
Embodiment 7
A kind of preparation method of cinnamon bark extract, comprises the following steps:
(1) cinnamon bark is crushed using medicinal herb grinder, crosses 60 mesh sieves, be dried to constant weight in 45 DEG C, obtain xylocinnamomum Skin powder;
(2) (cinnamon bark powder is mixed to cinnamon bark powder using ether:The mass ratio of ether is 1:60), stir 1h, filtering, is dried to constant weight in 45 DEG C by filter residue, obtains degreasing cinnamon bark powder;Weight is recovered by distillation in ether in filtrate It is multiple to utilize;
(3) in a reservoir, the ethanol water and 1.5g degreasing cinnamon bark powder for being 60% by 120mL percentage by volumes Mixing, sealing, with 720W ultrasonic power ultrasonic extraction 1.5h under conditions of 60 DEG C, filtering, filtrate stratification, it is clear to remove layer At night, obtain cinnamon bark crude extract;The content of tannic acid is 91.3mg/g in cinnamon bark crude extract, and the content of flavones is 172.1mg/g;
(4) cinnamon bark crude extract being concentrated under reduced pressure, (- 0.1MPa vacuum, rotary speed 115rpm/min, evaporation are warm 45 DEG C of degree, 2 DEG C of circulating condensing temperature), frozen dried (- 78 DEG C of cryogenic temperature, cooling time 48h, vacuum pressure 20Pa), obtain The powdered cinnamon bark crude extracts of 0.27g;
(5) use volume fraction that powdered cinnamon bark crude extract is dissolved into (ethanol for 10% ethanol water The aqueous solution and the amount ratio of cinnamon bark crude extract are 100mL:1g), obtain redissolving liquid;Liquid will be redissolved and use D101 macropore trees Fat gel column purifies, and is that eluent is eluted using volume fraction as 75% ethanol water, eluate depressurize dense Contract (- 0.1MPa vacuum, rotary speed 115rpm/min, 45 DEG C of evaporating temperature, 2 DEG C of circulating condensing temperature), frozen dried is (cold Freeze -78 DEG C of temperature, cooling time 48h, vacuum pressure 20Pa), obtain cinnamon bark extract after purification.Purified in the present embodiment The weight/mass percentage composition of tannic acid is 31.11% in cinnamon bark extract afterwards, and the weight/mass percentage composition of flavones is 93.62%.Tannin acid content reaches 31.11% in the present embodiment, is improved than cinnamon bark crude extract tannin acid content 49.04%, flavones content after purification reaches 93.62% (mass fraction), improves 64.21%.
Comparative example 1
A kind of preparation method of cinnamon bark crude extract, comprises the following steps:
(1) cinnamon bark is crushed using medicinal herb grinder, crosses 60 mesh sieves, be dried to constant weight in 45 DEG C, obtain xylocinnamomum Skin powder;
(2) (cinnamon bark powder is mixed to cinnamon bark powder using ether:The mass ratio of ether is 1:60), stir 1h, filtering, is dried to constant weight in 45 DEG C by filter residue, obtains degreasing cinnamon bark powder;Weight is recovered by distillation in ether in filtrate It is multiple to utilize;
(3) in a reservoir, the ethanol water and 1.5g degreasing cinnamon bark powder for being 60% by 120mL percentage by volumes Mixing, sealing, 1.5h is extracted with 0W ultrasonic powers under conditions of 60 DEG C, filtering, filtrate stratification, a layer stillness of night is removed, obtains To cinnamon bark crude extract.
The content for determining tannic acid in cinnamon bark crude extract is 74.6mg/g, and the content of chromocor extract is 130.9mg/ g。
Comparative example 2
A kind of preparation method of cinnamon bark extract, comprises the following steps:
(1) cinnamon bark is crushed using medicinal herb grinder, crosses 60 mesh sieves, be dried to constant weight in 45 DEG C, obtain xylocinnamomum Skin powder;
(2) (cinnamon bark powder is mixed to cinnamon bark powder using ether:The mass ratio of ether is 1:60), stir 1h, filtering, is dried to constant weight in 45 DEG C by filter residue, obtains degreasing cinnamon bark powder;Weight is recovered by distillation in ether in filtrate It is multiple to utilize;
(3) in a reservoir, the ethanol water and 1.5g degreasing cinnamon bark powder for being 60% by 120mL percentage by volumes Mixing, sealing, with 720W ultrasonic power ultrasonic extraction 1h under conditions of 60 DEG C, filtering, filtrate stratification, it is clear to remove layer At night, obtain cinnamon bark crude extract;The content of tannic acid is 90.5mg/g in cinnamon bark crude extract, and the content of flavones is 170.7mg/g;
(4) cinnamon bark crude extract being concentrated under reduced pressure, (- 0.1MPa vacuum, rotary speed 115rpm/min, evaporation are warm 45 DEG C of degree, 2 DEG C of circulating condensing temperature), frozen dried (- 78 DEG C of cryogenic temperature, cooling time 48h, vacuum pressure 20Pa), obtain powder Last shape cinnamon bark crude extract;
(5) use volume fraction that powdered cinnamon bark crude extract is dissolved into (ethanol for 10% ethanol water The aqueous solution and the amount ratio of cinnamon bark crude extract are 100mL:1g), obtain redissolving liquid;Liquid will be redissolved and use D101 macropore trees Fat gel column purifies, and is that eluent is eluted using volume fraction as 75% ethanol water, eluate depressurize dense Contract (- 0.1MPa vacuum, rotary speed 115rpm/min, 45 DEG C of evaporating temperature, 2 DEG C of circulating condensing temperature), frozen dried is (cold Freeze -78 DEG C of temperature, cooling time 48h, vacuum pressure 20Pa), obtain cinnamon bark extract after purification.Purified in the present embodiment The weight/mass percentage composition of tannic acid is 31.06% in cinnamon bark extract afterwards, and the weight/mass percentage composition of flavones is 92.58%.
It is horizontal as five factor three using the concentration of ethanol water, solid-to-liquid ratio, Extracting temperature, extraction time and extraction power, From L18(37) 18 groups of orthogonal tests of orthogonal arrage, by orthogonal test analysis, for the extraction process of cinnamon bark crude extract The concentration of ethanol water, solid-to-liquid ratio, Extracting temperature, extraction power are key factors in five factors, and extraction time is insignificant Factor, the extraction efficiency of embodiment 7 are best.
Embodiment 7 understands that ultrasonic extraction carries than traditional extraction process with recovery rate result in the crude extract of comparative example 1 Take rate much higher, the recovery rate of tannic acid adds 22.4%, and the recovery rate of flavones adds 31.5%.It can be seen that ultrasound carries The production technology of cinnamon bark extract is taken, extraction efficiency can be greatly improved, it is cost-effective, meet the requirement of green production.
The result of embodiment 7 and comparative example 2 understands, extraction time influences and little on the extraction efficiency of cinnamomum cassia extract, It is consistent with the interpretation of result of orthogonal test.
High extraction efficiency, relatively low extraction time, it is clear that the characteristics of meeting ultrasonic extraction, by the technique of ultrasonic extraction It is applied in the extraction of cinnamomum cassia extract, it is clear that meet the requirement of large-scale production.
Using gel column purifying when, macroreticular resin in extract active ingredient purifying tool have a certain impact, now with Prepared by embodiment 7 redissolves influence of the liquid investigation macroreticular resin to the adsorption-desorption ability of active ingredient:
(1) ten kinds of macroreticular resins are chosen:Be respectively D101, D4020, HPD-100, DM130, AB-8, S-8, ADS-17, DA-201C, HPD-400 and MAK- II;
(2) macroreticular resin is conventionally pre-processed, by the macroreticular resin 3.0g and cinnamon bark of pretreatment Crude extract redissolves liquid 90ml mixing, sealing, gently shakes up dispersion resin, stands 24 hours, filtering, the supernatant liquor of filtrates tested In tannic acid and flavones concentration, both concentration are lower, illustrate that the adsorption capacity of the macroreticular resin is stronger;
(3) ethanol water that 60ml volume fractions are 75% is added into the macroreticular resin after filtering, is sealed, 12 hours Fully desorption, filtering afterwards, clear liquid test tannic acid and flavones concentration are taken, both concentration are higher, illustrate the desorption of the macroreticular resin Ability is stronger.
The redissolution liquid active ingredient adsorption capacity test result that ten kinds of macroreticular resins are prepared to embodiment 7 is as shown in table 1, solution Energy-absorbing power test result is as shown in table 2.
10 kinds of macroreticular resins of table are to redissolving liquid active ingredient adsorption capacity test result
Desorption ability test result after 20 kinds of macroporous resin adsorption active ingredients of table
Resin Tannic acid desorbs absorbance Flavones desorbs absorbance
D101 0.488 0.616
D4020 0.465 0.581
HPD-100 0.479 0.599
DM130 0.461 0.565
AB-8 0.448 0.510
S-8 0.449 0.533
ADS-17 0.414 0.473
DA-201C 0.420 0.471
HPD-400 0.432 0.512
MAK-Ⅱ 0.279 0.265
It was found from Tables 1 and 2, cinnamon bark crude extract is purified from D101 macroreticular resins, to tannic acid or flavones Absorption and desorption have a quite excellent performance, therefore the present invention carries out purifying selected macropore to cinnamon bark crude extract The preferred D101 macroreticular resins of resin.
The present invention passes through the tannic acid and flavone mixture in ultrasonic extraction cinnamon bark, whole technical process operation letter Single, the production time is shorter, and recovery rate is higher.When the process conditions using embodiment 7,1.0kg cinnamon bark, can obtain pure The common 83.7g of cinnamon bark extract after change, productivity effect are high.
Performance test:Phenoxyethanol (dosage is added in the cinnamon bark extract after purification prepared to 0.1g embodiments 7 For cinnamon bark extract quality 0.5%), add mass concentration be 25% the butanediol aqueous solution, be settled to 100mL, shake Even fully dissolving, obtains cinnamon bark extract test fluid.The PH of the aqueous solution containing 10% test fluid is 7.03, the test fluid Electrical conductivity be 17.4 μ s/cm.Heat-resisting cold-resistant test 6 months is carried out at 45 DEG C and -18 DEG C, fever and chills are handed at 45 DEG C and -18 DEG C For 6 months, illumination 6 months, cinnamon bark extract test fluid was stable, and without Precipitation, color smell is significant change. In summary, cinnamon bark extract after purification can be used as composition the effect of cosmetics to be applied in Cosmetic Manufacture.
Efficacy test:Cinnamon bark extract test fluid is subjected to efficacy test, mainly including anti-oxidant test and whitening Test, its method of testing and result are as follows:Cinnamon bark extract test fluid:The xylocinnamomum after purification prepared to embodiment 7 Phenoxyethanol (dosage is the 0.5% of cinnamon bark extract quality) is added in bark extract, it is 25% to add mass concentration The butanediol aqueous solution, is settled to 100mL, shakes up abundant dissolving;
(1) anti-oxidant test
1. DPPH clearance rates determine
20mgDPPH accurately is weighed, with methanol constant volume to 500mL, obtains 0.04mg/mL mother liquors (DPPH solution);Take 0.2mL Cinnamon bark extract test fluid (concentration 0,0.1,0.2,0.3,0.5,0.6,0.8,1mg/mL) adds in 20mL test tubes The above-mentioned DPPH solution of 7.8ml, after reacting 30min under the conditions of lucifuge, light absorption value is surveyed under the conditions of 517nm, is obtained dense with sample introduction It is A=20.536c-0.0106 (R to the equation of linear regression of absorbance (A) to spend (c)2=0.999 9).According to standard curve DPPH concentration in sample after calculating reaction.(S is blank to DPPH clearance rate in foundation formula Y=(S-N)/S*100 calculating samples DPP concentration in sample, N are DPPH concentration in sample).Test result is as shown in table 3.
The DPPH clearance rates of the cinnamon bark extract test fluid of the various concentrations of table 3
2. FRAP methods survey total antioxidation value
FRAP working solution matching while using:The acetate buffer that by 25mL concentration be 300mmol/L and PH is 3.6,2.5mL Concentration is 10mmol/L TPTZ solution, and 2.5mL concentration is 20mmol/L FeCl3Solution mixes.
The FeSO of certain gradient concentration is drawn respectively4Titer 0.1mL, 3mL FRAP working solutions are added, are added 0.3mL ultra-pure waters, are mixed, accurate response 5min, and its light absorption value is determined at 593nm, is returned to zero with ultra-pure water, and it is bent to draw standard Line, by the above method using sample introduction concentration (c) to the equation of linear regression of absorbance (A) as A=0.5975c+0.0311 (r= 0.999 9)。
The measure of sample:Measure 0.1mL various concentrations cinnamon bark extract test fluid (concentration 0.1,0.2, 0.3rd, 0.5,0.6,0.8,1mg/mL), the total antioxidation value of determination sample in the above conditions.Test result is as shown in table 4.
The anti-oxidant value of the cinnamon bark extract test fluid of the various concentrations of table 4
It was found from table 3 and table 4, cinnamon bark extract of the invention has extremely strong anti-oxidation efficacy, need to only add dense Spend for 0.3mg/mL when, you can reach preferable antioxidant effect, DPPH free radical scavenging activities reach 98.30%, oxidation FeSO of the ability equivalent to 2.10mmol/L4, continue to increase the concentration of cinnamon bark extract, the clearance rate contribution to DPPH is not Greatly, it can be understood as free radical scavenging activity only up to reach 98.30%, but its oxidation resistance is still correspondingly improved. In summary, cinnamon bark extract of the invention, under extremely low addition, you can there is very high oxidation resistance, Free radical can be effectively removed, there is good senile-resistant efficacy.
(2) whitening is tested
Formed respectively by the reaction solution of table 5 with micropipettor, accurately draw TYR, the PBS in T1, T2, T3, T4 Buffer solution and cinnamon bark extract test fluid, it is placed in 4 PE pipes (being respectively designated as T1, T2, T3, T4), mixes, 37 DEG C of perseverances Warm 10min, 1mL tyrosinase is then separately added into T2, T4, reacts 10min, quickly existed with ultraviolet specrophotometer Its absorbance A is determined at 475nmT1、AT2、AT3、AT4.The activity that sample suppresses tyrosinase is calculated as follows:Tyrosinase Maximum inhibition=[1- (AT4-AT3)/(AT2-AT1)] × 100% wherein, AT1:Product are not loaded and do not add the reaction of tyrosinase The absorbance that liquid measures at 475nm, AT2:The product of not being loaded do not add absorbance of the reaction solution of tyrosinase at 475nm, AT3:Add Sample and plus tyrosinase the absorbance that is measured at 475nm of reaction solution, AT4:Sample-adding product and the reaction solution for adding tyrosinase The absorbance measured at 475nm.Reaction solution composition is as shown in table 5, and test result is as shown in table 6.
The reaction solution of table 5 forms
The whitening test result table of table 6
As can be known from Table 6, cinnamon bark extract of the invention can play a part of to suppress tyrosinase, although with addition The increase of amount, the inhibiting rate of tyrosinase remain to rise, but when addition is more than 0.3mg/mL, it appears that peak value is had arrived at, this The cinnamon bark extract of invention has whitening effect.
Using:Cinnamon bark extract prepared by embodiment 7 is used for the emulsion for preparing O/W:
Application Example 1
Stearine 1.0g, PEG-100 stearate 0.5g, white oil 6g, 16/18 alcohol 1.5g, polydimethylsiloxanes Alkane 1g, C10-18 resin acid triglyceride 2g, Nipasol 0.1g, glycerine 2g, butanediol 5g, methyl hydroxybenzoate 0.2g, allantoin 0.1g, AVC 0.2g, cinnamon bark extract 0.01g, add distilled water to 100g, mark It is designated as No. 1 emulsion.
Application Example 2
With Application Example 1, difference is that cinnamon bark extract is 0.03g, labeled as No. 2 emulsions.
Application Example 3
With Application Example 1, difference is that cinnamon bark extract is 0.05g, labeled as No. 3 emulsions.
Application Example 4
With Application Example 1, difference is that cinnamon bark extract is 0.10g, labeled as No. 4 emulsions.
Comparative example 5
With Application Example 1, difference is that cinnamon bark extract is 0g, labeled as No. 5 emulsions.
From 50 trial volunteers, security test, both effectiveness is carried out to Application Example 1~4 and comparative example 5 Test and stability test.
(1) security test
Patch test is carried out to 50 volunteers, because the skin of inboard arm is more tender and lovely, therefore selected inside arm The patch test that five regions carry out 1-5 emulsions is selected, the testing time is 24 hours, records test process and result, its result As shown in table 7:
The sample patch security test result of table 7
Sample It is rubescent Heating Shouting pain Allergy
No. 1 emulsion Nothing Nothing Nothing Nothing
No. 2 emulsions Nothing Nothing Nothing Nothing
No. 3 emulsions Nothing Nothing Nothing Nothing
No. 4 emulsions Nothing Nothing Nothing Nothing
No. 5 emulsions Nothing Nothing Nothing Nothing
(2) both effectiveness test
50 volunteers are divided into 5 groups, every group of 10 people, corresponds to use 1-5 emulsions 2 months respectively, after preceding use Respectively take pictures test and self-assessment test, record brilliant white degree, color spot area percentage are carried out with face-image analyzer VISIA-CR Than (color spot area selects area ratio with cutting), wrinkle area percentage (wrinkle area selects area ratio with cutting) and pachylosis Degree, test result are as shown in table 8:
The sample efficacy assessments of table 8
(3) stability test
Heat-resisting cold-resistant test 6 months, alternation of chills and fever 6 months, illumination 6 at 45 DEG C and -18 DEG C are carried out at 45 DEG C and -18 DEG C Individual month, 1-5 emulsion-stabilizings, without water-oil separating, viscosity, color, smell were significant change.
In summary, the cinnamon bark extract that the present invention extracts is added in cosmetics, does not influence the stabilization of cosmetics Property, it is safe and non-stimulating, and anti-ageing whitening effect can be provided, it is a kind of efficient, safe, green cosmetic material.The present invention Extracting method is efficient, extraction time is short, product high efficiency, is adapted to large-scale production.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification, Equivalent substitute mode is should be, is included within protection scope of the present invention.

Claims (10)

  1. A kind of 1. preparation method of cinnamon bark extract, it is characterised in that:Comprise the following steps:
    (1) cinnamon bark is crushed, sieved, drying, obtain cinnamon bark powder;
    (2) ungrease treatment is carried out to cinnamon bark powder using solvent, filtering, filter residue is dried, obtains degreasing cinnamon bark powder End;
    (3) ethanol water is mixed with degreasing cinnamon bark powder, the ultrasonic extraction under conditions of 30~70 DEG C, filtered, filter Liquid stratification, takes subnatant, obtains cinnamon bark crude extract;
    (4) cinnamon bark crude extract is concentrated under reduced pressure, frozen dried, obtains powdered cinnamon bark crude extract;
    (5) volume fraction is used to be dissolved cinnamon bark crude extract for 5%~15% ethanol water, then using macropore Resin gel post is purified, and is that eluent is eluted using volume fraction as 30%~90% ethanol water, and eluate is entered Row is concentrated under reduced pressure, and freezes, obtains cinnamon bark extract after purification.
  2. 2. the preparation method of cinnamon bark extract according to claim 1, it is characterised in that:
    The percentage by volume of ethanol is 0~80% in ethanol water described in step (3);Degreasing Chinese cassia tree described in step (3) The mass volume ratio of bark fines and ethanol water is (1.0~6.0) g:120mL;The work(of ultrasonic extraction described in step (3) Rate is 0~800W;The temperature of ultrasonic extraction described in step (3) is 40 DEG C~60 DEG C.
  3. 3. the preparation method of cinnamon bark extract according to claim 2, it is characterised in that:Ethanol described in step (3) The percentage by volume of ethanol is 40%~80% in the aqueous solution;Degreasing cinnamon bark powder and ethanol are water-soluble described in step (3) The mass volume ratio of liquid is 1g:(40~80) mL;The power of ultrasonic extraction described in step (3) is 400~800W.
  4. 4. the preparation method of cinnamon bark extract according to claim 1, it is characterised in that:Step elutes described in (5) Liquid is that volume fraction is 75% ethanol water.
  5. 5. the preparation method of cinnamon bark extract according to claim 1, it is characterised in that:Macropore described in step (5) The potting resin of resin gel post is D101, D4020, HPD-100, DM130, AB-8, S-8, ADS-17, DA-201C, HPD- One kind in 400 and MAK- II.
  6. 6. the preparation method of cinnamon bark extract according to claim 1, it is characterised in that:Chinese cassia tree described in step (5) The volume ratio of volume and gel column after the dissolving of bark crude extract is 1:15~1:40;
    The ratio between the post footpath of macroreticular resin gel column and pillar height are 1:40~1:85;
    When being purified using macroreticular resin gel column, loading flow velocity is 1.0-6.0ml/min.
  7. 7. the preparation method of cinnamon bark extract according to claim 1, it is characterised in that:Step holds agent described in (2) For petroleum ether, ether or ethyl acetate, the mass ratio of the cinnamon bark powder and solvent is 1:(10~100);The degreasing The condition of processing is that 0.5~5h is stirred under normal temperature.
  8. 8. the preparation method of cinnamon bark extract according to claim 1, it is characterised in that:Step is dried described in (1) Temperature be 40~50 DEG C;The temperature dried described in step (2) is 40~50 DEG C;Ultrasonic extraction described in step (3) when Between be 0.25~2.5h;
    The condition being concentrated under reduced pressure described in step (5) is:Temperature is 40~50 DEG C, and rotary speed is 100~120rpm.
  9. 9. a kind of cinnamon bark extract is obtained as the preparation method described in any one of claim 1~8.
  10. 10. the application of cinnamon bark extract according to claim 1, it is characterised in that:The cinnamon bark extract is used In the cosmetics for preparing anti-aging and/or whitening.
CN201710970697.9A 2017-10-18 2017-10-18 A kind of cinnamon bark extract and preparation method thereof and the application in cosmetics Pending CN107496269A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109007785A (en) * 2018-09-26 2018-12-18 上饶市康可得生物科技有限公司 A kind of auxiliary hyperglycemic blood fat reducing healthcare food
CN110664865A (en) * 2019-10-18 2020-01-10 中国林业科学研究院林产化学工业研究所 Method for separating and preparing extract of cinnamon steaming oil residues and application of extract
CN110711164A (en) * 2019-11-27 2020-01-21 广东工业大学 Extraction method and application of cinnamon extracting solution
CN111888290A (en) * 2020-08-18 2020-11-06 广东丸美生物技术股份有限公司 Cinnamon bark extract and preparation method and application thereof
CN115192631A (en) * 2022-08-29 2022-10-18 北京明阳华夏科技有限公司 Preparation method of cinnamon extract, cinnamon extract and application of cinnamon extract

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102872195A (en) * 2012-11-05 2013-01-16 天津市聚星康华医药科技有限公司 Preparation method of cinnamon total polyphenol extract and application thereof
CN103584254A (en) * 2013-11-19 2014-02-19 广东嘉豪食品股份有限公司 Preparation method for aseptic containing compound clove/cinnamon extracts and aseptic application of aseptic in sauce products
CN106417562A (en) * 2016-11-25 2017-02-22 防城港市畜牧站 Biological fresh keeping agent for aquatic products
CN106974002A (en) * 2017-05-18 2017-07-25 马鞍山市京友调味品有限公司 A kind of soybean oil containing complex natural antioxidant and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102872195A (en) * 2012-11-05 2013-01-16 天津市聚星康华医药科技有限公司 Preparation method of cinnamon total polyphenol extract and application thereof
CN103584254A (en) * 2013-11-19 2014-02-19 广东嘉豪食品股份有限公司 Preparation method for aseptic containing compound clove/cinnamon extracts and aseptic application of aseptic in sauce products
CN106417562A (en) * 2016-11-25 2017-02-22 防城港市畜牧站 Biological fresh keeping agent for aquatic products
CN106974002A (en) * 2017-05-18 2017-07-25 马鞍山市京友调味品有限公司 A kind of soybean oil containing complex natural antioxidant and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
陈荟芸: "肉桂单宁提取分离纯化及抗氧化活性研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109007785A (en) * 2018-09-26 2018-12-18 上饶市康可得生物科技有限公司 A kind of auxiliary hyperglycemic blood fat reducing healthcare food
CN110664865A (en) * 2019-10-18 2020-01-10 中国林业科学研究院林产化学工业研究所 Method for separating and preparing extract of cinnamon steaming oil residues and application of extract
CN110711164A (en) * 2019-11-27 2020-01-21 广东工业大学 Extraction method and application of cinnamon extracting solution
CN111888290A (en) * 2020-08-18 2020-11-06 广东丸美生物技术股份有限公司 Cinnamon bark extract and preparation method and application thereof
CN115192631A (en) * 2022-08-29 2022-10-18 北京明阳华夏科技有限公司 Preparation method of cinnamon extract, cinnamon extract and application of cinnamon extract

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Application publication date: 20171222