CN106691937A - Forsythia flower extract for inhibiting tyrosinase, and preparation method thereof and application - Google Patents

Forsythia flower extract for inhibiting tyrosinase, and preparation method thereof and application Download PDF

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Publication number
CN106691937A
CN106691937A CN201710003219.0A CN201710003219A CN106691937A CN 106691937 A CN106691937 A CN 106691937A CN 201710003219 A CN201710003219 A CN 201710003219A CN 106691937 A CN106691937 A CN 106691937A
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CN
China
Prior art keywords
capsule
flower extract
weeping forsythia
tyrosinase
extract
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CN201710003219.0A
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Chinese (zh)
Inventor
张立伟
李石飞
李丹凤
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Shanxi University
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Shanxi University
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Priority to CN201710003219.0A priority Critical patent/CN106691937A/en
Publication of CN106691937A publication Critical patent/CN106691937A/en
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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
    • 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

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Veterinary Medicine (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Biotechnology (AREA)
  • Engineering & Computer Science (AREA)
  • Dermatology (AREA)
  • Botany (AREA)
  • Microbiology (AREA)
  • Mycology (AREA)
  • Birds (AREA)
  • Epidemiology (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
  • Cosmetics (AREA)

Abstract

The invention provides a forsythia flower extract for inhibiting tyrosinase, and a preparation method thereof and application. The forsythia flower extract is prepared by making forsythia flower undergo extraction by a hydrophilic solvent and preparing and separating effective ingredients through column chromatography. In the extract, the content of total flavonoids is over 12.0%, and the IC50 value of inhibiting tyrosinase activity is 0.67 mg/mL and is close to 0.52 mg/mL of the IC50 value of arbutin inhibiting tyrosinase. Since tyrosinase is a key enzyme for synthesizing melanin, the extract has good tyrosinase inhibiting activity, the extract has a potential beauty effect against chloasma and malar rash and the like caused by melanin pigmentation abnormity and can be applied to cosmetic development.

Description

Capsule of weeping forsythia flower extract and its preparation method and application for suppressing tyrosinase
Technical field
The present invention relates to cosmetic technical field, specifically a kind of capsule of weeping forsythia flower extract for suppressing tyrosinase and its Preparation method and application.
Background technology
Chloasma, the butterfly macules of human face belong to melanin pigmentation and cause extremely, and tyrosinase is synthesis of melanin Key enzyme, by suppressing the bioactivity of tyrosinase, can indirectly suppress the generation of melanin.Therefore, current nti-freckle, Main component is with the kojic acid with suppression tyrosinase activity, based on ursin in skin-lightening cosmetic.And from natural plants Middle screening tyrosinase inhibitor is simultaneously applied to the focus that always cosmetics are studied in nti-freckle, skin-lightening cosmetic.Such as aloe, sweet The extract of grass and mulberry tree is used widely in nti-freckle, skin-lightening cosmetic.
Flos Forsythiae is the flower of the Oleaceae forsythia capsule of weeping forsythia, containing the biological flavone composition such as abundant rutin, and is had Stronger anti-oxidant and antibacterial activity.And among the people with the custom drunk as jasmine tea using Flos Forsythiae.
The content of the invention
It is an object of the invention to provide a kind of capsule of weeping forsythia flower extract for suppressing tyrosinase and preparation method thereof and Using.
A kind of preparation method for suppressing the capsule of weeping forsythia flower extract of tyrosinase that the present invention is provided, including following step Suddenly:
(1) extract:Weigh a certain amount of capsule of weeping forsythia dried flower, crush, add 8~10 times of hydrophilic solvents of amount, be standing and soak for 30min, 1~2h of refluxing extraction, filtering, residue is again with 8~10 times of hydrophilic solvent refluxing extraction 1h of amount, filtering, merging two Secondary extract solution, 60 DEG C are concentrated under reduced pressure into the Flos Forsythiae concentrate that proportion is 1.05~1.10;
(2) separate:Concentrate is washed with deionized water de- 2 first further with non-polar column chromatographic material chromatography ~4 column volumes, then with 20%, 40%, 60% ethanol water successively respectively elute 2~4 column volumes, collect 60% second The eluent of alcohol solution, is concentrated under reduced pressure, dries, and obtains capsule of weeping forsythia flower extract.
Hydrophilic solvent described in step (1) can be that the mixing of the water and ethanol of water, ethanol, methyl alcohol or different proportion is molten Agent, the water of different proportion and the mixed solvent of methyl alcohol, preferably use 70% ethanol water.
Non-polar column chromatographic material described in step (2) can be C18With MDS-5 any one.
Effective constituent determination:Using NaNO2-A1(NO3)3General flavone content in-NaOH colorimetric method for determining active components, The content of general flavone (general flavone content is calculated with rutin equivalent) more than 12.0% in the active component of Flos Forsythiae.
Capsule of weeping forsythia flower extract with above-mentioned acquisition, can be with carrier, other beauty-care activity components, diluent as active component Etc. being mixed and made into the specific functionality cosmetics such as toner, emulsion, condensation, facial mask and face cream.
The invention has the advantages that:Flos Forsythiae extractive total flavone content prepared by the present invention is (total for more than 12.0% Flavones content is calculated with rutin equivalent).Capsule of weeping forsythia flower extract suppresses the IC of tyrosinase activity50It is 0.67mg/mL to be worth, and suppresses effect Fruit is suitable with ursin, and (ursin suppresses the IC of tyrosinase50Value 0.52mg/mL).It can be answered in nti-freckle, skin-lightening cosmetic With.
Specific embodiment
With reference to specific embodiment, the present invention is furture elucidated.
Embodiment 1 weighs 100g capsules of weeping forsythia dried flower, the appropriate ethanol water crushed, add 1000mL 70%, stands leaching Bubble 30min, refluxing extraction 1h, filtering, residue is again with the ethanol water refluxing extraction 1h of 1000mL 70%, filtering, merging two Secondary filtrate, it is 1.05 to be concentrated under reduced pressure into concentrate proportion.Concentrate is further with nonpolar C18Column chromatography material chromatography, First it is washed with deionized water de- 3 column volumes, then 3 column volumes is respectively eluted successively with 20%, 40%, 60% ethanol water, Deionized water and 20%, 40% ethanol water wash-out liquid are discarded, the eluent of 60% ethanol water is collected, depressurized dense Contract, dry, obtain capsule of weeping forsythia flower extract.In the capsule of weeping forsythia flower extract content of general flavone be 12.5% (general flavone content with rutin work as Amount is calculated).
Embodiment 2 weighs 100g capsules of weeping forsythia dried flower, the appropriate ethanol water crushed, add 800mL 70%, is standing and soak for 30min, refluxing extraction 1.5h, filtering, residue is again with the ethanol water refluxing extraction 1h of 800mL 70%, filtering, merging two Secondary filtrate, it is 1.10, recycling design to be concentrated under reduced pressure into concentrate proportion.Concentrate is further with nonpolar MDS-5 column chromatographies Material chromatography, is first washed with deionized water de- 4 column volumes, then is eluted successively with 20%, 40%, 60% ethanol water 4 column volumes, discard deionized water and 20%, 40% ethanol water wash-out liquid, and the ethanol water for collecting 60% is washed It is de-, it is concentrated under reduced pressure, dries, obtain capsule of weeping forsythia flower extract.The content of general flavone is 12.7% (general flavone content in capsule of weeping forsythia flower extract Calculated with rutin equivalent).
In vitro test of the capsule of weeping forsythia flower extract of embodiment 3 to the inhibitory action of tyrosinase
The capsule of weeping forsythia flower extract prepared by embodiment 1 observes the inhibitory action to tyrosinase
Tyrosinase inhibition test system is as described in Table 1.During experiment, first add Mushroom Tyrosinase (TYR) and difference The capsule of weeping forsythia flower extract and ursin solution of concentration, 10min is preheated at 37 DEG C, is eventually adding the μ L of substrate TYR 20, is triggered Reaction, setting Detection wavelength is 475nm, absorbance during record 30min.Every group of experiment is in triplicate.
Tyrosinase inhibition rate computing formula is:I%={ [(A-B)-(C-D)]/(A-B) } × 100%
Capsule of weeping forsythia flower extract is shown in Table 2 to the histamine result of Mushroom Tyrosinase.Illustrate that the Flos Forsythiae of present invention acquisition is extracted Thing is close with ursin to the inhibition of Mushroom Tyrosinase activity, with stronger inhibition.
The tyrosinase inhibitory activity of table 1 tests reaction system
The IC50 that the capsule of weeping forsythia flower extract of table 2 suppresses to Mushroom Tyrosinase

Claims (7)

1. a kind of preparation method for suppressing the capsule of weeping forsythia flower extract of tyrosinase, it is characterised in that comprise the following steps:
(1) extract:Weigh a certain amount of capsule of weeping forsythia dried flower, crush, add 8~10 times of hydrophilic solvents of amount, be standing and soak for 30min, 1~2h of refluxing extraction, filtering, residue with 8~10 times of hydrophilic solvent refluxing extraction 1h of amount, is filtered again, and merging is extracted twice Liquid, 60 DEG C are concentrated under reduced pressure into the Flos Forsythiae concentrate that proportion is 1.05~1.10;
(2) separate:Concentrate is washed with deionized water de- 2~4 first further with non-polar column chromatographic material chromatography Column volume, then with 20%, 40%, 60% ethanol water successively respectively elute 2~4 column volumes, collect 60% ethanol water The eluent of solution, is concentrated under reduced pressure, dries, and obtains capsule of weeping forsythia flower extract.
2. a kind of preparation method for suppressing the capsule of weeping forsythia flower extract of tyrosinase as claimed in claim 1, its feature exists In the hydrophilic solvent described in step (1) is water, ethanol, methyl alcohol, ethanol water or methanol aqueous solution.
3. a kind of preparation method for suppressing the capsule of weeping forsythia flower extract of tyrosinase as claimed in claim 1, its feature exists In the ethanol water is 70% ethanol water.
4. a kind of preparation method for suppressing the capsule of weeping forsythia flower extract of tyrosinase as claimed in claim 1, its feature exists In the non-polar column chromatographic material described in step (2) can be C18Or MDS-5.
5. such as the capsule of weeping forsythia flower extract of claim 1-4 either method preparation.
6. application of the capsule of weeping forsythia flower extract as claimed in claim 5 in nti-freckle, skin-lightening cosmetic is prepared.
7. a kind of nti-freckle, skin-lightening cosmetic, contain capsule of weeping forsythia flower extract as claimed in claim 5 in its component.
CN201710003219.0A 2017-01-03 2017-01-03 Forsythia flower extract for inhibiting tyrosinase, and preparation method thereof and application Pending CN106691937A (en)

Priority Applications (1)

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CN201710003219.0A CN106691937A (en) 2017-01-03 2017-01-03 Forsythia flower extract for inhibiting tyrosinase, and preparation method thereof and application

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CN201710003219.0A CN106691937A (en) 2017-01-03 2017-01-03 Forsythia flower extract for inhibiting tyrosinase, and preparation method thereof and application

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2023129732A1 (en) * 2021-12-31 2023-07-06 Laboratory Corporation Of America Holdings Methods and systems for hydrophilic-phase extraction

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103193836A (en) * 2013-04-19 2013-07-10 山东农业大学 Method for separating and purifying monomers in forsythia suspensa flower
CN106053704A (en) * 2016-05-09 2016-10-26 山东农业大学 A rapid analysis method for a fructus forsythiae flower chemical component fingerprint

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103193836A (en) * 2013-04-19 2013-07-10 山东农业大学 Method for separating and purifying monomers in forsythia suspensa flower
CN106053704A (en) * 2016-05-09 2016-10-26 山东农业大学 A rapid analysis method for a fructus forsythiae flower chemical component fingerprint

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2023129732A1 (en) * 2021-12-31 2023-07-06 Laboratory Corporation Of America Holdings Methods and systems for hydrophilic-phase extraction

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