CN111973532B - Saffron extract for treating skin acne and application thereof - Google Patents

Saffron extract for treating skin acne and application thereof Download PDF

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CN111973532B
CN111973532B CN202010940279.7A CN202010940279A CN111973532B CN 111973532 B CN111973532 B CN 111973532B CN 202010940279 A CN202010940279 A CN 202010940279A CN 111973532 B CN111973532 B CN 111973532B
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CN111973532A (en
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刘金平
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Guangzhou Keying Cosmetic Co ltd
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    • 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]
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • A61P17/10Anti-acne agents
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    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
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    • A61K2236/30Extraction of the material
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    • A61K2236/333Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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    • A61K2236/50Methods involving additional extraction steps
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    • 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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Abstract

The invention discloses a saffron extract for treating skin acne, which is prepared by the following steps: (1) cleaning saffron crocus, drying, and grinding to 60-100 meshes to obtain saffron crocus powder; (2) preparing an extraction solution, adding saffron crocus powder into the extraction solution, carrying out ultrasonic treatment, filtering, and removing filter residues to obtain a filtrate 1; (3) placing the filtrate 1 in a water bath at 50-70 ℃, centrifuging after the water bath, and obtaining a supernatant; (4) adding the supernatant into 50-70% ethanol, further extracting in microwave extraction equipment, filtering, and removing filter residues to obtain a filtrate 2; (5) and (4) decompressing and concentrating the filtrate 2 obtained in the step (4), adjusting the pH value to 6.4-6.8, and drying in vacuum to obtain the saffron extract. The saffron extract for treating skin acne has a good effect of treating acne, and has wide application in cosmetics.

Description

Saffron extract for treating skin acne and application thereof
Technical Field
The invention relates to the field of cosmetics, and in particular relates to a saffron extract for treating skin acne and application thereof.
Background
Saffron, also known as saffron and crocus, is a perennial flower of crocus of iridaceae, is also an aromatic plant, is an original seed in southwest asia, has the first artificial greek cultivation, and is mainly planted in Shanghai, Zhejiang, Henan, Hubei and the like in China at present. Saffron is a famous and precious Chinese medicinal material, and is recorded in Ben Cao gang mu: has neutral nature and sweet taste, and has effects of dredging meridian passage, nourishing blood, replenishing blood, removing blood stasis, relieving swelling and pain, cooling blood, removing toxic substances, resolving stagnation, tranquilizing mind, regulating qi-flowing, and invigorating stomach. Modern scientific researches prove that the saffron has the pharmacological effects of resisting mental disorders such as depression and anxiety, treating the neurodegenerative diseases such as premenstrual syndrome, Parkinson's disease, Alzheimer disease and the like, the cerebrovascular diseases such as cerebral infarction, cerebral ischemia and cerebral trauma and the like, the cardiovascular diseases such as myocardial ischemia and hypertrophy and the like, improving learning and memory disorders, resisting atherosclerosis, regulating blood fat and resisting diabetes, and also has the pharmacological effects of enhancing immunity, reducing low-density lipoprotein, cholesterol and the like. Saffron belongs to edible natural spice which is allowed to be used in China, can be used for drinks, wine blending and the like, and has good food therapy and health care effects.
Acne is a chronic inflammatory disease of the sebaceous gland structure of the hair follicle, mainly occurs on the face and the back, and is manifested by comedones, inflammatory papules, secondary pustules or nodules, cysts and the like.
Acne is commonly known as comedo, pimple or whelk, is one of the most common skin diseases, is clinically manifested as chronic skin inflammation, not only affects the skin health of patients, but also easily affects the psychology, social contact and the like of the patients, particularly teenagers. At present, most of the medicines for treating acne are antibiotics, have poor treatment effect and toxic and side effects, cannot be used for a long time, and can cause certain damage to facial skin.
Disclosure of Invention
The invention provides a saffron extract for treating skin acne and application thereof, wherein the saffron extract has the function of treating skin acne and has wide application in cosmetics.
The invention adopts the following technical scheme for solving the technical problems:
a saffron extract for treating skin acne is prepared by the following steps:
(1) cleaning saffron crocus, drying, and grinding to 60-100 meshes to obtain saffron crocus powder;
(2) preparing an extraction solution, adding saffron crocus powder into the extraction solution, carrying out ultrasonic treatment, filtering, and removing filter residues to obtain a filtrate 1;
(3) placing the filtrate 1 in a water bath at 50-70 ℃, centrifuging after the water bath, and obtaining a supernatant;
(4) adding the supernatant into 50-70% ethanol, further extracting in microwave extraction equipment, filtering, and removing filter residues to obtain a filtrate 2;
(5) and (4) decompressing and concentrating the filtrate 2 obtained in the step (4), adjusting the pH value to 6.4-6.8, and drying in vacuum to obtain the saffron extract.
As a preferred scheme, dissolving the saffron extract by using distilled water with the volume of 2-5 times, then carrying out chromatography treatment, eluting by using ethyl acetate-methanol-deionized water with the elution amount of 2-4 BV, collecting eluent, adding anhydrous ethanol with the volume of 3-5 times into the eluent for alcohol precipitation, standing for 4-6 h, centrifuging to obtain precipitates, and carrying out vacuum drying to obtain the purified saffron extract.
The inventor of the invention finds that the saffron extract is processed by chromatography in a large number of saffron extraction and purification experiments, and a series of parameters and extract raw materials which are applicable to the saffron extract are defined, so that the more purified saffron extract is prepared, and the skin acne can be more effectively treated.
As a preferred embodiment, the chromatography is performed using a DEAE Sepharose column.
Preferably, the extraction solution is a 15-30% ammonium sulfate solution and 40-70% ethanol according to a volume ratio of 1: 1-2 mixing.
As a most preferred embodiment, the extraction solution is a 25% ammonium sulfate solution and 50% ethanol at a volume ratio of 1: 1.8 mixing.
When the inventor of the present invention finds a suitable extraction solution for the saffron extract, the inventor of the present invention has unexpectedly found that a more pure saffron extract can be obtained by mixing an ammonium sulfate solution and ethanol as the extraction solution, and the extract has a higher crocin content.
As a preferable scheme, the weight ratio of the saffron crocus powder to the extraction solution is 1: 15-25.
As a preferable scheme, the weight ratio of the supernatant to the ethanol is 1: 4 to 8.
As a preferable scheme, the ultrasonic treatment time is 25-40 min, and the power is 300-500W.
As a preferable scheme, the microwave extraction time is 20-40 min, and the microwave frequency is 800-900 MHz.
As a preferred scheme, the saffron extract for treating skin acne is used for preparing cosmetics for treating acne.
The invention has the beneficial effects that: (1) the saffron extract for treating skin acne has good effect of treating acne and wide application in cosmetics; (2) the saffron extract is extracted by the extraction solution, is subjected to chromatography treatment, and is subjected to DEAE sepharose column and ethyl acetate-methanol-deionized water as eluent to obtain the saffron extract with good acne treatment effect; (3) the saffron extract has high content of crocin, wherein the content of crocin can be improved by chromatographic treatment, eluent selection and extraction solution selection.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are a part of the embodiments of the present invention, but not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A saffron extract for treating skin acne is prepared by the following steps:
(1) cleaning stigma croci Sativi, drying, and grinding to 90 mesh to obtain stigma croci Sativi powder;
(2) preparing an extraction solution, adding saffron crocus powder into the extraction solution, carrying out ultrasonic treatment, filtering, and removing filter residues to obtain a filtrate 1;
(3) placing the filtrate 1 in a water bath at 60 ℃, centrifuging after the water bath, and obtaining supernatant;
(4) adding the supernatant into 60% ethanol, further extracting in microwave extraction equipment, filtering, and removing the filter residue to obtain filtrate 2;
(5) and (4) concentrating the filtrate 2 obtained in the step (4) under reduced pressure, adjusting the pH value to 6.5, and drying in vacuum to obtain the saffron extract.
The extraction solution is a 25% ammonium sulfate solution and 50% ethanol according to a volume ratio of 1: 1.8 mixing.
The weight ratio of the saffron powder to the extraction solution is 1: 24.
The weight ratio of the supernatant to the ethanol is 1: 5.
the ultrasonic treatment time is 35min, and the power is 450W.
The microwave extraction time is 30min, and the microwave frequency is 900 MHz.
Example 2
A saffron extract for treating skin acne is prepared by the following steps:
a saffron extract for treating skin acne is prepared by the following steps:
(1) cleaning stigma croci Sativi, drying, and grinding to 90 mesh to obtain stigma croci Sativi powder;
(2) preparing an extraction solution, adding saffron crocus powder into the extraction solution, carrying out ultrasonic treatment, filtering, and removing filter residues to obtain a filtrate 1;
(3) placing the filtrate 1 in a water bath at 60 ℃, centrifuging after the water bath, and obtaining supernatant;
(4) adding the supernatant into 60% ethanol, further extracting in microwave extraction equipment, filtering, and removing the filter residue to obtain filtrate 2;
(5) and (4) concentrating the filtrate 2 obtained in the step (4) under reduced pressure, adjusting the pH value to 6.5, and drying in vacuum to obtain the saffron extract.
Dissolving the saffron extract by using distilled water with the volume of 4 times, then carrying out chromatography treatment, eluting by using ethyl acetate-methanol-deionized water with the elution amount of 2.5BV, collecting eluent, adding absolute ethyl alcohol with the volume of 4 times into the eluent for alcohol precipitation, standing for 4h, centrifuging to obtain precipitate, and carrying out vacuum drying to obtain the purified saffron extract.
The chromatography is carried out by using a DEAE sepharose column.
The extraction solution is a 25% ammonium sulfate solution and 50% ethanol according to a volume ratio of 1: 1.8 mixing.
The weight ratio of the saffron powder to the extraction solution is 1: 24.
The weight ratio of the supernatant to the ethanol is 1: 5.
the ultrasonic treatment time is 35min, and the power is 450W.
The microwave extraction time is 30min, and the microwave frequency is 900 MHz.
Example 3
A saffron extract for treating skin acne is prepared by the following steps:
(1) cleaning stigma croci Sativi, drying, and grinding to 100 mesh to obtain stigma croci Sativi powder;
(2) preparing an extraction solution, adding saffron crocus powder into the extraction solution, carrying out ultrasonic treatment, filtering, and removing filter residues to obtain a filtrate 1;
(3) placing the filtrate 1 in a water bath at 70 ℃, centrifuging after the water bath, and obtaining supernatant;
(4) adding the supernatant into 70% ethanol, further extracting in microwave extraction equipment, filtering, and removing the filter residue to obtain filtrate 2;
(5) and (4) concentrating the filtrate 2 obtained in the step (4) under reduced pressure, adjusting the pH value to 6.8, and drying in vacuum to obtain the saffron extract.
The extraction solution is a 25% ammonium sulfate solution and 50% ethanol according to a volume ratio of 1: 1.8 mixing.
The weight ratio of the saffron crocus powder to the extraction solution is 1: 15-25.
The extraction solution is a 25% ammonium sulfate solution and 50% ethanol according to a volume ratio of 1: 1.8 mixing.
The weight ratio of the saffron powder to the extraction solution is 1: 24.
The weight ratio of the supernatant to the ethanol is 1: 5.
the ultrasonic treatment time is 35min, and the power is 450W.
The microwave extraction time is 30min, and the microwave frequency is 900 MHz.
Example 4
A saffron extract for treating skin acne is prepared by the following steps:
(1) cleaning stigma croci Sativi, drying, and grinding to 100 mesh to obtain stigma croci Sativi powder;
(2) preparing an extraction solution, adding saffron crocus powder into the extraction solution, carrying out ultrasonic treatment, filtering, and removing filter residues to obtain a filtrate 1;
(3) placing the filtrate 1 in a water bath at 70 ℃, centrifuging after the water bath, and obtaining supernatant;
(4) adding the supernatant into 70% ethanol, further extracting in microwave extraction equipment, filtering, and removing the filter residue to obtain filtrate 2;
(5) and (4) concentrating the filtrate 2 obtained in the step (4) under reduced pressure, adjusting the pH value to 6.8, and drying in vacuum to obtain the saffron extract.
Dissolving the saffron extract by using distilled water with the volume of 4 times, then carrying out chromatography treatment, eluting by using ethyl acetate-methanol-deionized water with the elution amount of 2.5BV, collecting eluent, adding absolute ethyl alcohol with the volume of 4 times into the eluent for alcohol precipitation, standing for 4h, centrifuging to obtain precipitate, and carrying out vacuum drying to obtain the purified saffron extract.
The extraction solution is a 25% ammonium sulfate solution and 50% ethanol according to a volume ratio of 1: 1.8 mixing.
The weight ratio of the saffron crocus powder to the extraction solution is 1: 15-25.
The extraction solution is a 25% ammonium sulfate solution and 50% ethanol according to a volume ratio of 1: 1.8 mixing.
The weight ratio of the saffron powder to the extraction solution is 1: 24.
The weight ratio of the supernatant to the ethanol is 1: 5.
the ultrasonic treatment time is 35min, and the power is 450W.
The microwave extraction time is 30min, and the microwave frequency is 900 MHz.
Comparative example 1
Comparative example 1 differs from example 1 in that the extraction solution described in comparative example 1 differs from example 1, all the other things being equal.
The extraction solution was the same as the 25% ammonium sulfate solution alone, except that it was used.
Comparative example 2
Comparative example 2 is different from example 2 in that comparative example 2 was eluted with chloroform-methanol, and the others were the same.
To further demonstrate the effect of the present invention, the following test methods were provided:
adding the saffron crocus extracts of the embodiments 1-4 and the comparative examples 1-2 into a cosmetic mask to prepare the mask, wherein in order to avoid influencing experimental results, conventional substances which do not treat skin acne are added into the mask formula, 120 volunteers with obvious acne of 18-25 years old are respectively selected, the mask is respectively tried, 1 tablet is used every night, no other cosmetics are used in the period, and after the mask is continuously tried for 14 days, the effect is observed, wherein: the acne subsides 90% for the basic recovery, subsides 60-89% for effectual, subsides 30-59% for effective, subsides 30% below for ineffective, and the test result is shown in table 1, wherein the formula of the facial mask is: 95.1 parts of deionized water, 0.05 part of disodium ethylene diamine tetraacetate, 4 parts of glycerin, 0.5 part of saffron extract, 0.25 part of xanthan gum and 0.1 part of preservative.
TABLE 1 test results
Figure DEST_PATH_IMAGE001
As can be seen from Table 1, the saffron extract of the present invention has good effect of treating acne on skin, wherein, the best proposal is shown in example 2, and the chromatography treatment can effectively improve the effect of treating the acne on the skin by comparing the example 1 with the example 2, comparing example 3 with example 4, it can be seen that the chromatography treatment is effective in improving the effect of treating acne on skin, comparing example 1 with comparative example 1, it can be seen that the selection of the extraction solution has a certain effect of improving the effect of treating acne on the skin, wherein the extraction solution of the invention is selected to improve the effect of treating skin acne, and as can be seen from comparative example 2 and comparative example 2, the selection of the eluent has a certain effect on improving the effect of treating the skin acne, wherein the selection of the eluent can improve the effect of treating the skin acne.
2. The content of crocin in the saffron extract described in examples 1-4 and comparative examples 1-2, and the test results are shown in table 2.
TABLE 2 content of crocin
Figure 212536DEST_PATH_IMAGE002
As can be seen from table 2, the content of crocin in the crocin extract of the present invention is high, as can be seen from comparative examples 1 and 2, the chromatography can effectively increase the content of crocin, as can be seen from comparative examples 3 and 4, the chromatography can effectively increase the content of crocin, as can be seen from comparative examples 1 and 1, the selection of the extraction solution has a certain effect on the content of crocin, wherein the selection of the extraction solution of the present invention can increase the content of crocin, as can be seen from comparative examples 2 and 2, the selection of the eluent has a certain effect on increasing the content of crocin, wherein the selection of the eluent of the present invention can increase the content of crocin.
In light of the foregoing description of preferred embodiments according to the invention, it is clear that many changes and modifications can be made by the person skilled in the art without departing from the scope of the invention. The technical scope of the present invention is not limited to the contents of the specification, and must be determined according to the scope of the claims.

Claims (3)

1. The saffron extract for treating skin acne is characterized in that the preparation method of the saffron extract comprises the following steps:
(1) cleaning saffron crocus, drying, and grinding to 60-100 meshes to obtain saffron crocus powder;
(2) preparing an extraction solution, adding saffron crocus powder into the extraction solution, carrying out ultrasonic treatment, filtering, and removing filter residues to obtain a filtrate 1;
(3) placing the filtrate 1 in a water bath at 50-70 ℃, centrifuging after the water bath, and obtaining a supernatant;
(4) adding the supernatant into 50-70% ethanol, further extracting in microwave extraction equipment, filtering, and removing filter residues to obtain a filtrate 2;
(5) concentrating the filtrate 2 obtained in the step (4) under reduced pressure, adjusting the pH value to 6.4-6.8, and drying in vacuum to obtain a saffron extract;
(6) dissolving the saffron extract by using distilled water with the volume of 2-5 times, then carrying out chromatography treatment by using a DEAE (DEAE) sepharose column, eluting by using ethyl acetate-methanol-deionized water, wherein the elution amount is 2-4 BV, collecting eluent, adding anhydrous ethanol with the volume of 3-5 times into the eluent for alcohol precipitation, standing for 4-6 h, centrifuging to obtain precipitate, and carrying out vacuum drying to obtain a purified saffron extract;
the extraction solution is a 25% ammonium sulfate solution and 50% ethanol according to a volume ratio of 1: 1.8 mixing;
the weight ratio of the saffron powder to the extraction solution is 1: 24; the ultrasonic treatment time is 35min, and the power is 450W; the microwave extraction time is 30min, and the microwave frequency is 900 MHz.
2. Saffron extract for the treatment of skin acne according to claim 1, wherein the weight ratio of said supernatant to ethanol is 1: 4 to 8.
3. Use of saffron extract for the treatment of acne on the skin according to any one of claims 1 to 2 for the preparation of a cosmetic for the treatment of acne.
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CN112826878A (en) * 2021-02-08 2021-05-25 陈应荣 Formula of crocus sativus skin-care and mucous membrane-protecting product and preparation method thereof
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CN115261142A (en) * 2022-08-29 2022-11-01 西藏天虹科技股份有限责任公司 Saffron extraction process and device

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