CN111388381A - Cosmetic elsholtzia extract and extraction method thereof - Google Patents

Cosmetic elsholtzia extract and extraction method thereof Download PDF

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Publication number
CN111388381A
CN111388381A CN202010434575.XA CN202010434575A CN111388381A CN 111388381 A CN111388381 A CN 111388381A CN 202010434575 A CN202010434575 A CN 202010434575A CN 111388381 A CN111388381 A CN 111388381A
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Prior art keywords
extract
liquid
resin
extracting
ethanol
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杨江勇
袁强
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Chengdu Beilekang Biotechnology Co ltd
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Chengdu Beilekang 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
    • A61K8/96Cosmetics 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
    • A61K8/9783Angiosperms [Magnoliophyta]
    • A61K8/9789Magnoliopsida [dicotyledons]
    • 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
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/34Alcohols
    • A61K8/347Phenols
    • 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
    • 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
    • A61Q17/02Barrier 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 containing insect repellants
    • 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
    • A61K2800/80Process 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

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Dermatology (AREA)
  • Epidemiology (AREA)
  • Birds (AREA)
  • Pest Control & Pesticides (AREA)
  • Plant Pathology (AREA)
  • Emergency Medicine (AREA)
  • Engineering & Computer Science (AREA)
  • Biotechnology (AREA)
  • Botany (AREA)
  • Microbiology (AREA)
  • Mycology (AREA)
  • Gerontology & Geriatric Medicine (AREA)
  • Cosmetics (AREA)

Abstract

The invention discloses an elsholtzia extract for cosmetics and an extraction method, wherein the elsholtzia extract for cosmetics contains: thymol is not less than 7.0 wt%, carvacrol is not less than 4.0 wt%, and total flavone is not less than 3 wt%, wherein the sum of thymol, carvacrol and total flavone is less than 100 wt%. The cosmetics prepared by the elsholtzia extract have stable color and no odor.

Description

Cosmetic elsholtzia extract and extraction method thereof
Technical Field
The invention belongs to the field of cosmetics, and particularly relates to an elsholtzia extract for cosmetics and an extraction method.
Background
Herba Moslae is dry aerial part of Moslachinismax or Mosla chinensis 'Jiiangxiangru' of Labiatae. The former is called Qingxiang hai she, the latter is called Jiang xiang hai she. Collecting and cutting in sunny days when stems and leaves are flourishing and flowers are flourishing in summer, removing impurities, and drying in the shade. It is commonly used for summer-damp common cold, aversion to cold, fever, headache, anhidrosis, abdominal pain, vomiting and diarrhea. The contents of the Chinese pharmacopoeia 2015 and the catalog of used cosmetic raw materials are recorded.
Modern researches show that the main effective components of the elsholtzia comprise volatile oil, flavonoid glycoside, organic acid glycoside and the like, wherein the content of the volatile oil is more than 0.6 percent in pharmacopoeia, the volatile oil mainly comprises thymol, carvacrol, thymol acetate, carvacrol acetate, α -caryophyllene and the like, the content of the volatile oil is more than 99 percent, the flavonoid mainly comprises luteolin, apigenin, baicalein-7-methyl ether and the like, and the organic acid mainly comprises chlorogenic acid, caffeic acid and the like.
The elsholtzia extract has the efficacy of A and antibiosis, and a plurality of reports report that elsholtzia volatile oil has stronger broad-spectrum antibacterial action, and the antibacterial active ingredients of the elsholtzia extract comprise thymol, carvacrol, p-cymene, caryophyllene oxide, luteolin, quercetin, 4-terpineol and the like, and the elsholtzia extract has certain antibacterial and bactericidal activity on typhoid bacillus, staphylococcus aureus, enteritis bacillus and escherichia coli. B. The elsholtzia volatile oil has obvious inhibition and killing effects on the expansion of cotton aphid population, and the effect of killing cotton aphids is better than acetamiprid wettable powder and abamectin emulsifiable solution; C. the elsholtzia haichowensis contains flavonoid compounds which have electrophilic capability and can remove free radicals and prevent chain reaction, thereby inhibiting lipid from being overoxidized.
A process for preparing the extract of Chinese mosla herb (201310746669.0) includes microwave heating while extracting in solvent, and features that the Chinese mosla herb extract is not enriched and purified, resulting in unstable color and smell.
Microwave extraction is an advanced and efficient extraction technology, and the extracted product has chemical component difference with the traditional alcohol extraction.
Method for extracting and separating pseudoschizonepeta glycoside, homoplantarin and apigenin glycoside from Elsholtzia splendens-201510582357. X; 105218605B, describes a method for separating monomeric pseudoschizonepeta glycosides, homoplantaginosides and apigenin glycosides from elsholtzia.
Elsholtzia extract and its preparation process and application-201410238435 describes the preparation process of Elsholtzia extract and its composition. The elsholtzia extract is not purified.
A method for comprehensively extracting volatile oil, polysaccharide and flavone from Elsholtzia splendens (lour.) Moss-201310391507. X describes a comprehensive utilization method of Elsholtzia splendens, which well utilizes various components in Elsholtzia splendens. There are also problems with unpurification in the aforementioned patents. A Chinese medicine in the form of dripping pill for treating the diseases caused by cold injury, etc is prepared from the extract of Chinese mosla herb through liquid paraffin and talc powder 200510004992.6. Patent method for extracting and separating rosmarinic acid, apigenin and luteolin from elsholtzia haichowensis-201310042896.5 describes a method for separating monomer rosmarinic acid, apigenin and luteolin. Is not suitable for industrialized production. A method for preparing herba Moslae essential oil, CN201310344665.X, describes a supercritical extraction method of herba Moslae oil with CO2, which is a high-quality oil extraction method, and the preparation principle is essentially different from the present patent.
Disclosure of Invention
Aiming at the defects, the invention provides the elsholtzia extract for cosmetics, which has the characteristics of stable quality, industrial production, high product conversion rate, low cost, low energy consumption and the like.
The technical scheme is as follows: an elsholtzia extract for cosmetics, which contains:
thymol is more than or equal to 7.0 wt%
The content of carvacrol is more than or equal to 4.0 wt%
The total flavone content is greater than or equal to wt 3%, wherein the total content of thymol, carvacrol and total flavone is less than 100 wt%.
The cosmetic prepared from herba Moslae extract has stable color and no odor.
The invention also provides an extraction method of the elsholtzia extract for cosmetics.
A method for extracting herba Moslae extract for cosmetic comprises the following steps:
① pulverizing herba Moslae;
② extracting with ethanol;
③ concentrating the extractive solution by molecular distillation;
④ diluting with water;
⑤ centrifuging to remove impurities;
⑥ adsorbing with macroporous resin, and eluting with ethanol;
⑦ decolorizing the eluate with resin, and collecting the decolorized liquid;
⑧ deproteinizing the decolorized liquid with resin to obtain deproteinized liquid containing ammonia and nitrogen;
⑨ concentrating ammonia nitrogen liquid such as deproteinized liquid with membrane;
⑩ concentrating the concentrated solution with molecular distillation concentrator, and drying to obtain light yellow white extract.
The method can be used for industrial production, and has the advantages of high product conversion rate, low cost and low energy consumption.
The elsholtzia extract extracted by the invention has stable quality, can be industrially produced, has the characteristics of high product conversion rate, low cost, low energy consumption and the like, is used for producing cosmetics, and the produced cosmetics have stable color and no odor.
Explanation and glossary of terms
In the present invention,% means mass% unless otherwise specified.
Detailed Description
The present invention will be further explained below.
A method for extracting herba Moslae extract for cosmetic comprises the following steps:
① pulverizing herba Moslae.
② extracting with ethanol.
③ and concentrating the extracted liquid by molecular distillation.
④ diluting with water.
⑤ centrifugation removes impurities.
⑥ macroporous resin is adsorbed and then eluted by ethanol.
⑦ decolorizing the eluate with resin, and collecting the decolorized liquid.
⑧ the decolorized liquid is deproteinized with resin to collect the deproteinized liquid.
⑨ the liquid containing ammonia nitrogen such as deproteinized liquid is concentrated with membrane.
⑩ concentrating the concentrated solution with molecular distillation concentrator, and drying to obtain light yellow white extract.
Example 1
Pulverizing 200g herba Moslae raw material (dry aerial part of herba Moslae) into 10-60 mesh, extracting with 70% ethanol at 75-80 deg.C for three times, concentrating the extractive solution by molecular distillation to remove ethanol to obtain 150ml concentrated solution, diluting with hot water for 2 times, centrifuging to remove impurities, adsorbing with EVR-1# macroporous resin (EVR-1# is type and volume is 150ml), eluting with 80% ethanol, decolorizing the eluate with D285 resin (D285 resin volume is 100ml), collecting decolorized liquid, removing ammonia nitrogen such as protein with D001 resin (D001 volume is 100ml), collecting liquid of ammonia nitrogen such as protein, concentrating with molecular distillation concentrator, concentrating, and drying to obtain light yellow white extract 6.5 g. Through detection, the content of thymol in the light yellowish white extract is 6.5%, the content of carvacrol is 4.2%, and the content of total flavonoids is 3%.
Example 2
Pulverizing herba Moslae raw material 200g to 10-60 mesh, extracting with 80% ethanol at 45-50 deg.C for three times, subjecting the extractive solution to molecular distillation and concentration until no alcohol is obtained to obtain 200ml of concentrated solution, diluting with hot water for 2 times, centrifuging to remove impurities, adsorbing with EVR-1# macroporous resin (EVR-1# type, volume 150ml), eluting with 80% ethanol, decolorizing the eluate with D285 resin (D285 resin volume is 100ml), collecting decolorized liquid, removing ammonia nitrogen such as protein with D001 resin (D001 resin volume is 100ml), collecting liquid of ammonia nitrogen such as protein, concentrating with molecular distillation concentrator, concentrating, and drying to obtain light yellow white extract 6.3 g. Through detection, the content of thymol in the light yellowish white extract is 5.5%, the content of carvacrol is 3.2%, and the content of total flavonoids is 3.5%.
Example 3
Pulverizing herba Moslae raw material 200g to 10-60 mesh, extracting with 80% ethanol at 75-80 deg.C for three times, subjecting the extractive solution to molecular distillation and concentration to remove ethanol to obtain 160ml of concentrated solution, diluting with hot water for 2 times, centrifuging to remove impurities, adsorbing with EVR-1# macroporous resin (EVR-1# is type, volume is 150ml), eluting with 80% ethanol, decolorizing the eluate with D285 resin (D285 resin volume is 100ml), collecting decolorized liquid, removing ammonia nitrogen compounds such as protein with D001 resin (D001 resin volume is 100ml), collecting liquid of ammonia nitrogen compounds such as protein, concentrating with molecular distillation concentrator, concentrating, and drying to obtain light yellow white extract 7.2g, which contains thymol 7.2%, carvacrol 3.7%, and total flavone 3.2%.
Example 4
Pulverizing herba Moslae raw material 200g to 10-60 mesh, extracting with 90% ethanol at 75-80 deg.C for three times, subjecting the extractive solution to molecular distillation and concentration until no alcohol is obtained to obtain 150ml concentrated solution, diluting with hot water for 2 times, centrifuging to remove impurities, adsorbing with EVR-1# macroporous resin (EVR-1# type, volume 150ml), eluting with 80% ethanol, decolorizing the eluate with D285 resin (D285 resin volume is 100ml), collecting decolorized liquid, removing ammonia nitrogen compounds such as protein with D001 resin (D001 resin volume is 100ml), collecting liquid of ammonia nitrogen compounds such as protein, concentrating with molecular distillation concentrator, concentrating, and drying to obtain light yellow white extract 7.4g, which contains thymol 7.5%, carvacrol 4.2%, and total flavone 3%.
Comparative example 1
Pulverizing 200g herba Moslae raw material (dry aerial parts of herba Moslae) into 10-60 mesh, extracting with 70% ethanol at 75-80 deg.C for three times, concentrating the extractive solution by molecular distillation to remove ethanol to obtain 150ml concentrated solution, diluting with hot water 2 times, centrifuging to remove impurities, adsorbing with EVR-1# macroporous resin (EVR-1# type, volume 150ml), eluting with 80% ethanol, concentrating the eluate, and drying to obtain brown yellow extract 10.2g, which contains 4.8% thymol, 2.8% carvacrol and 2.1% total flavonoids.
The light yellow extract extracted in examples 1-4 of the present invention and the brown yellow extract extracted in comparative example 1 were used for the production of cosmetics, respectively, and the cosmetics produced in examples 1-4 were stable in color and free of odor.
Sample (I) Case 1 Case 2 Case 3 Case 4 Comparative example 1
Concentration of sample 1% 1% 1% 1% 1%
Thermal stabilization Light yellow Light yellow Light yellow Light yellow Yellow colour
Cold stabilization Light yellow Light yellow Light yellow Light yellow Yellow, hasPrecipitation of
The pH8 is stable Yellowish Yellowish Yellowish Yellowish Yellow colour
The pH5 is stable Light yellow Light yellow Light yellow Light yellow Yellow colour
Illumination stabilization Yellowish Yellowish Yellowish Yellowish Yellow colour
Long-term stability for 30 days Light yellow Light yellow Light yellow Light yellow Yellow colour
Note: sample concentration samples were dissolved in water containing 30% ethylene glycol.
Thermal stability conditions: and (5) performing constant temperature culture in a 40 +/-1 incubator for 48 hours.
Cold stability conditions: in a refrigerating chamber at 3 +/-1 ℃ for 48 hours
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (3)

1. An elsholtzia extract for cosmetics, which contains:
thymol is more than or equal to 7.0 wt%
The content of carvacrol is more than or equal to 4.0 wt%
The total flavone content is greater than or equal to wt 3%, wherein the total content of thymol, carvacrol and total flavone is less than 100 wt%.
2. A method for extracting herba Moslae extract for cosmetic comprises the following steps:
① pulverizing herba Moslae;
② extracting with ethanol;
③ concentrating the extractive solution by molecular distillation;
④ diluting with water;
⑤ centrifuging to remove impurities;
⑥ adsorbing with macroporous resin, and eluting with ethanol;
⑦ decolorizing the eluate with resin, and collecting the decolorized liquid;
⑧ deproteinizing the decolorized liquid with resin to obtain deproteinized liquid containing ammonia and nitrogen;
⑨ concentrating ammonia nitrogen liquid such as deproteinized liquid with membrane;
⑩ concentrating the concentrated solution with molecular distillation concentrator, and drying to obtain light yellow white extract.
3. The method for extracting herba Moslae extract for cosmetics according to claim 2, wherein the extract is obtained by pulverizing herba Moslae to 10-60 mesh in ①, extracting 70-80% ethanol in ② at 45-50 deg.C in ③.
CN202010434575.XA 2020-05-21 2020-05-21 Cosmetic elsholtzia extract and extraction method thereof Pending CN111388381A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113425635A (en) * 2021-05-10 2021-09-24 江苏省中国科学院植物研究所 Elsholtzia extract, its preparation and use

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103695181A (en) * 2013-12-31 2014-04-02 湖南省百里香天然生物制品开发有限公司 Preparation method of elsholtziae extract
CN104312729A (en) * 2014-10-23 2015-01-28 湖南省百里香天然生物制品开发有限公司 Extracting method of elsholtia containing 0.5% to 1.5% of thymol

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103695181A (en) * 2013-12-31 2014-04-02 湖南省百里香天然生物制品开发有限公司 Preparation method of elsholtziae extract
CN104312729A (en) * 2014-10-23 2015-01-28 湖南省百里香天然生物制品开发有限公司 Extracting method of elsholtia containing 0.5% to 1.5% of thymol

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113425635A (en) * 2021-05-10 2021-09-24 江苏省中国科学院植物研究所 Elsholtzia extract, its preparation and use

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Application publication date: 20200710