CN107496275A - Camellia seed washes clean stoste and preparation method thereof - Google Patents

Camellia seed washes clean stoste and preparation method thereof Download PDF

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Publication number
CN107496275A
CN107496275A CN201710973482.2A CN201710973482A CN107496275A CN 107496275 A CN107496275 A CN 107496275A CN 201710973482 A CN201710973482 A CN 201710973482A CN 107496275 A CN107496275 A CN 107496275A
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CN
China
Prior art keywords
camellia seed
stoste
washes clean
camellia
slag
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201710973482.2A
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Chinese (zh)
Inventor
赖琼玮
陈劲松
张俊天
杨耀学
黄闺
张帆
洪穗
成超丽
罗秋兰
吴丹
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Hunan Sanxiang Camellia Oil Agel Ecommerce Ltd
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Hunan Sanxiang Camellia Oil Agel Ecommerce Ltd
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Application filed by Hunan Sanxiang Camellia Oil Agel Ecommerce Ltd filed Critical Hunan Sanxiang Camellia Oil Agel Ecommerce Ltd
Priority to CN201710973482.2A priority Critical patent/CN107496275A/en
Publication of CN107496275A publication Critical patent/CN107496275A/en
Pending legal-status Critical Current

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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
    • A61Q17/00Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
    • A61Q17/005Antimicrobial preparations
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q5/00Preparations for care of the hair
    • A61Q5/006Antidandruff preparations
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q5/00Preparations for care of the hair
    • A61Q5/02Preparations for cleaning the hair
    • 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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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Engineering & Computer Science (AREA)
  • Biotechnology (AREA)
  • Botany (AREA)
  • Microbiology (AREA)
  • Mycology (AREA)
  • Birds (AREA)
  • Epidemiology (AREA)
  • Dermatology (AREA)
  • Cosmetics (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

A kind of camellia seed washes clean stoste and preparation method thereof, and its former technique is:(1)Squeezing:Tea seed is squeezed and obtains camellia seed slag;(2)Leach:By step(1)Camellia seed slag is obtained by extraction, obtains the camellia seed slag that deoils;(3)Crush:By step(2)The obtained camellia seed ground-slag that deoils is broken, sieving, obtains camellia seed powder;(4)Cold extraction:By step(3)Obtained camellia seed powder and deionized water proportionally mix, and after ultrasonic wave stirring, filter to get filtrate;(5)Chromatography:By step(4)The filtrate regulation pH of acquisition, stoste is obtained by chromatographing to filter;(6)It is refined:By step(5)The stoste regulation pH of acquisition, filtering obtain clarification camellia seed and wash clean stoste.The technique realizes the extraction skill of Tea Saponin in ancient method camellia seed, while causes the reservation of the benefit materials such as Tea Polyphenols contained therein, tea polysaccharide, and desensitizes completely so that camellia seed, which washes clean stoste, to be able to extensive use in Cosmetic Market.

Description

Camellia seed washes clean stoste and preparation method thereof
Technical field
The present invention relates to a kind of camellia seed to wash clean stoste and preparation method thereof, particularly a kind of camellia seed through desensitization process Wash clean stoste and preparation method thereof.
Background technology
The Aqueous extracts of teaseed cake dregs are a kind of abstersive cleaning suppliess of traditional tool in south China, wherein containing Tea Saponin be a kind of natural nonionic surfactant, there is the effect such as anti-inflammation and sterilization, can also be by teaseed cake dregs with water original In water soluble tea cake protein, the material original such as tea polysaccharide come out, long-term use have it is anti-dandruff, antipruritic, deoil, sterilize, the work(of black hair Effect, but its Aqueous extracts is applied can allergic phenomena in cosmetics, causes user's skin erythema, itch, its security is deposited In certain risk, therefore finding one kind can effectively desensitize, and the method that and can is effectively retained effectively nutritional ingredient therein, is to solve Camellia seed washes the unique channel of clean stoste application in cosmetics.
The content of the invention
The purpose of the present invention is to overcome existing camellia seed to wash clean stoste allergic problem, finds a kind of extraction that can effectively desensitize Method.
The technical scheme is that camellia seed washes the preparation method of clean stoste, in turn include the following steps:
(1)Squeezing:Tea seed is squeezed and obtains camellia seed slag;
(2)Leach:By step(1)Camellia seed slag is obtained by extraction, obtains the camellia seed slag that deoils;
(3)Crush:By step(2)The obtained camellia seed ground-slag that deoils is broken, sieving, obtains camellia seed powder;
(4)Cold extraction:By step(3)Obtained camellia seed powder and deionized water proportionally mix, after environment temperature stirring, filtering Obtain filtrate;
(5)Chromatography:By step(4)The filtrate regulation PH of acquisition, stoste is obtained by chromatographing to filter;
(6)It is refined:By step(5)The stoste regulation PH of acquisition, adds filter aid, is filtered by filter, obtain clarification camellia Seed washes clean stoste.
Wherein step(2)Described in solvent be n-hexane.
Wherein step(3)Described in camellia seed powder particles degree be the mesh of 30 mesh -100.
Wherein step(4)Described in camellia seed powder and deionized water mixed proportion be 1:(3-10), temperature is environment temperature Degree, mixing time are 20-40 minutes, and mixing speed is 20-60 revs/min.
Wherein step(4)It is middle to be stirred using ultrasonic wave, 500-2000 watts of described ultrasonic power, frequency 20-40KHz.
Wherein step(5)Described in regulation PH in 2-4, the acidity, which can be good at separating out, sensitizer and to be changed over time Caused muddy thing, is analysed after precipitation by silica gel sand bed, just adsorbs the material of this particle diameter very well.So that subsequent liquid is not present Allergy and long-time deposit muddy problem, influence subsequently to use.
Wherein step(5)Described chromatography media is husky using the mesh silica gel of 30 mesh -100, and filtering is using chromatography filtering, chromatography The 2-5% silica gel of paving filtrate weight is husky in tank.
Wherein step(6)Described regulation pH is in 5-6, it is therefore an objective to neutralization procedure(5)Acidity, the acidity can be good at melting The compounding of unclassified stores is closed, makes subsequent applications more extensive.
Wherein step(4)Described in filtering use sedimentation centrifuge.
Wherein step(5)Described in filtering use leaf-type filter.
Wherein step(6)Using filter aid diatomite, addition is the 1-6% of stoste weight.
The camellia seed obtained present invention additionally comprises above extracting method washes clean stoste.
Beneficial effects of the present invention are as follows:
1st, the technique realizes the skill of Tea Saponin in ancient method extraction camellia seed, while make it that Tea Polyphenols contained therein, tea are more The extraction of the benefit materials such as sugar, and desensitize completely so that mountain camellia seed, which washes clean stoste, to be able to extensive use in Cosmetic Market, Improve its security;
2nd, technique is simple, and thing heating engineering, whole cold extraction, energy consumption is low, and effect is good.
Primary raw material used in the present invention is described as follows:
Camellia seed:It is the fruit of tea oil tree;Tea oil tree is the main woody oleiferous plants tree in China, is described as " east tree ", belongs to camellia Section's Camellia evergreen dungarunga, it is the distinctive woody vegetable oil resource in China;3-6 meters of the height of tree, the diameter of a cross-section of a tree trunk 1.3 meters above the ground is up to 24-30 lis Rice, smooth bark is taupe;Tea oil tree list leaf alternate, flower are both sexes white, and October, Post flowering was until fruit between October next year Can be ripe, therefore, tea oil tree has rare flowers and fruits homophyletic phenomenon;Fruit is capsule, is mostly ellipse, has fine, soft fur;Seed Mostly yellowish-brown, glossy, triangular shape;Tea oil tree is grown in remote mountains, inhales natural nutrient to the greatest extent, evergreen longevity, the age of tree was up to 200 years More than.
Deionized water:Refer to eliminate the pure water in after ionic species impurity, International Organization for standardization ISO/TC 147 is advised Fixed " deionization " is defined as:" deionized water is complete or incompletely removes ionic species ", using the method system of RO counter-infiltrations Take, the anion and cation gone using ion exchange resin in water removal.
Embodiment
Embodiment 1
The camellia seed of embodiment 1 washes clean stoste, in turn includes the following steps:
(1)Squeezing:Tea seed is squeezed and obtains camellia seed slag;
(2)Leach:By step(1)Camellia seed slag is obtained by extraction, obtains the camellia seed slag that deoils;
(3)Crush:By step(2)The obtained camellia seed ground-slag that deoils is broken, is sieved through 60 eye mesh screens, obtains camellia seed powder;
(4)Cold extraction:By step(3)Obtained 1000 grams of camellia seed powder mixes for 6000 grams with deionized water, opens ultrasonic wave, power 500 watts, frequency 20KHz, after stirring 20min, sedimentation centrifuge filters to get filtrate 5510 grams;
(5)Chromatography:By step(4)The filtrate regulation pH of acquisition obtains 5460 grams of stoste 2, by chromatographing tank filtering;Chromatograph tank Interior paving filtrate 2%, the mesh silica gel of 30 mesh -100 are husky.
(6)It is refined:By step(5)The stoste regulation pH of acquisition adds filter aid, is filtered, obtained by leaf-type filter 5 Camellia seed must be clarified and wash clean 5412 grams of stoste.
Embodiment 2-6
Embodiment 2-6 camellia seed washes clean stoste process of preparing, and its preparation process condition is simply anti-substantially with embodiment 1 The condition such as raw material and proportion scale, temperature, time is answered to be slightly different, specifically as listed in table 1.
The embodiment 1-6 of table 1 camellia seed washes clean stoste preparation process condition
Clean stoste is washed according to the gained camellia seed of table 1 and carries out color and luster, active quantities and moist detection, the results are shown in Table 2.
The camellia seed of table 2 washes clean stoste and carries out color and luster, active quantities and moist detection
Note:- to no effect;+ slightly lubricate;++ lubrication;+++ lubricate very much
Color and luster influences cosmetic appearance, and yellowish-brown is natural tea seed color;Active matter content influences clean effect.
Embodiment 1-6 and comparative example 1-4 camellia seed are washed into clean stoste and carry out patch test, patch test results such as table 3 Row.
The camellia seed of table 3 washes clean stoste patch test results
Note:- without allergic reaction;± doubtful allergy;+ slight allergy;++ allergy;+++ severe allergy
Used method of testing is as follows in table 3:
Step 1:The gauze of four thickness is cut into a diameter of 1cm circle with scissors, totally 8, draws 25uL's respectively with liquid-transfering gun Camellia seed washes clean stoste, drops on circular gauze, and blank is done with deionized water;
Step 2:The gripping of gauze tweezers is placed on subject(Clean stoste allergy sufferers are washed to camellia seed)At anteflexion arm, use Adhesive tape fixes, and starts timing;
Step 3:Torn after 48h adhesive tape, and observe the reaction of skin at gauze covering immediately;Observe result such as table 3 above institute Show.
As can be seen from Table 3, the desensitization effect of embodiment is good, and washes most suitableization on clean stoste color and luster and activity in camellia seed Cosmetic application.
Relieving itching and removing dandruff anticreep tea seed hair washing juice toxicology test of the present invention through desensitization process:Skin irritation test(It is more Secondary skin irritation test).
Test objective:Observe rabbit intact skin long-time multiple-contact tested material(The camellia seed of the embodiment of the present invention is washed Clean stoste)Caused skin irritation reaction afterwards, wash clean stoste for the camellia seed of the embodiment of the present invention security foundation is provided.
Test basis:《Cosmetics health specification》Version in 2007;Test method:From white New Zealand rabbits 8, random point For 2 groups, every group 4;A groups:Experimental group, B groups:Deionized water control group.24h is by family's rabbit back backbone both sides hair before experiment Cut, do not damage skin surface in cropping, unhairing scope is 3cm × 3cm, and application area is 2.5cm × 2.5cm, tested material group Camellia seed to various embodiments of the present invention washes clean stoste, takes tested material 0.5ml to be coated directly on the side of back backbone, opposite side 0.5ml control group deionized waters are applied, smears 1 time daily, continuously smears 14d;Since second day, cropping when smearing every time, use Deionized water removes residual tested material;Result is observed after one hour, according to《Cosmetics health specification》The skin of version in 2007 Irritation test table is scored, and check plot and trial zone are equally handled.
Evaluation of result:Every rabbit average integral daily is calculated according to the following formula, is pierced by specification list deciding rabbit skin Swash intensity, and observe other toxic actions in addition to excitant.
Result of the test:Tested material was carried out in the multiple skin irritation test observation period, gave various embodiments of the present invention Through desensitize PROCESS FOR TREATMENT camellia seed wash clean stoste after, rabbit has no erythema, oedema;Have no systemic toxicity profiles performance and dead feelings Condition, the weight of animals increase, on breathing, circulating, central nervous system, four limbs activity etc. is without influence.
Conclusion (of pressure testing):The camellia seed through the PROCESS FOR TREATMENT that desensitizes of various embodiments of the present invention washes clean stoste to white New Zealand Rabbit intact skin is nonirritant.

Claims (10)

1. a kind of camellia seed washes clean stoste preparation method, comprise the following steps successively:
(1)Squeezing:Tea seed is squeezed and obtains camellia seed slag;
(2)Leach:By step(1)Camellia seed slag is obtained by extraction, obtains the camellia seed slag that deoils;
(3)Crush:By step(2)The obtained camellia seed ground-slag that deoils is broken, sieving, obtains camellia seed powder;
(4)Cold extraction:By step(3)Obtained camellia seed powder and deionized water proportionally mix, and open ultrasonic wave, after stirring, Filter to get filtrate;
(5)Chromatography:By step(4)The filtrate of acquisition, regulation pH value pass through and chromatograph filtering and obtain stoste in 2-4;
(6)It is refined:By step(5)The stoste regulation pH value of acquisition is added filter aid, filtered by filter, obtain mountain in 5-6 Tea seed washes clean stoste.
2. camellia seed according to claim 1 washes clean stoste preparation method, it is characterised in that step(2)Described in solvent For n-hexane.
3. camellia seed according to claim 1 washes clean stoste preparation method, it is characterised in that step(3)Described in camellia Seed powder particles degree is 30-100 mesh.
4. camellia seed according to claim 1 washes clean stoste preparation method, it is characterised in that step(4)Described in camellia Seed powder and deionized water mixed proportion are 1:(3-10), temperature is environment temperature, and mixing time is 20-40 minutes, mixing speed For 20-60 revs/min.
5. camellia seed according to claim 1 washes clean stoste preparation method, it is characterised in that step(4)It is middle to use ultrasonic wave Stirring, described ultrasonic wave, 500-2000 watts of power, frequency 20-40KHz.
6. camellia seed according to claim 1 washes clean stoste preparation method, it is characterised in that step(5)Described chromatography is situated between Matter is husky using the mesh silica gel of 30 mesh -100, is filtered by chromatographing tank, and the 2-5% silica gel of paving filtrate weight is husky in chromatography tank.
7. camellia seed according to claim 1 washes clean stoste preparation method, it is characterised in that step(4)Described in filtering Using sedimentation centrifuge.
8. camellia seed according to claim 1 washes clean stoste preparation method, it is characterised in that step(6)Described in filtering Using leaf-type filter.
9. camellia seed according to claim 1 washes clean stoste preparation method, it is characterised in that:The step(6)Using helping Filtering agent diatomite, addition are the 1-6% of stoste weight.
10. washing the camellia seed that clean stoste preparation method obtains using any camellia seeds of claim 1-9 washes clean stoste.
CN201710973482.2A 2017-10-18 2017-10-18 Camellia seed washes clean stoste and preparation method thereof Pending CN107496275A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110637836A (en) * 2019-09-29 2020-01-03 湖南粮食集团有限责任公司 Extraction method of nanoscale bacteriostatic camellia seed extract

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102372761A (en) * 2011-10-10 2012-03-14 安徽农业大学 Method for extracting tea saponin from sasanglla cake
CN102977162A (en) * 2012-12-17 2013-03-20 贵州泰谷农业科技有限公司 Method for producing high-purity tea saponin
CN104961793A (en) * 2015-06-29 2015-10-07 兰捷 Method for extracting high-purity tea saponin from tea seed cake dregs

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102372761A (en) * 2011-10-10 2012-03-14 安徽农业大学 Method for extracting tea saponin from sasanglla cake
CN102977162A (en) * 2012-12-17 2013-03-20 贵州泰谷农业科技有限公司 Method for producing high-purity tea saponin
CN104961793A (en) * 2015-06-29 2015-10-07 兰捷 Method for extracting high-purity tea saponin from tea seed cake dregs

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110637836A (en) * 2019-09-29 2020-01-03 湖南粮食集团有限责任公司 Extraction method of nanoscale bacteriostatic camellia seed extract
CN110637836B (en) * 2019-09-29 2021-05-14 湖南粮食集团有限责任公司 Extraction method of nanoscale bacteriostatic camellia seed extract

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Application publication date: 20171222