CN112870236A - Flavone effective part of abelmoschus manihot and preparation method and application thereof - Google Patents
Flavone effective part of abelmoschus manihot and preparation method and application thereof Download PDFInfo
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics 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
- A61K8/9783—Angiosperms [Magnoliophyta]
- A61K8/9789—Magnoliopsida [dicotyledons]
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P17/00—Drugs for dermatological disorders
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P17/00—Drugs for dermatological disorders
- A61P17/18—Antioxidants, e.g. antiradicals
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q17/00—Barrier 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
- A61Q17/04—Topical preparations for affording protection against sunlight or other radiation; Topical sun tanning preparations
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/004—Aftersun preparations
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/08—Anti-ageing preparations
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction 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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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/805—Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Abstract
The invention relates to a flavonoid effective part of abelmoschus manihot, a preparation method and application thereof, belonging to the field of medicines, wherein the flavonoid effective part of abelmoschus manihot comprises the following flavonoid components: the effective part of the abelmoschus manihot flavonoid has good effects of preventing or treating skin aging, repairing and resisting aging, and the effective part of the abelmoschus manihot flavonoid has the advantages of being capable of preventing or treating skin aging, repairing and resisting aging, and being capable of preventing and treating skin aging, and preventing skin aging.
Description
Technical Field
The invention belongs to the field of medicines, particularly relates to a flavonoid effective part of abelmoschus manihot and a preparation method and application thereof, and particularly relates to a high-purity flavonoid effective part of abelmoschus manihot prepared by a membrane separation coupling resin method and application thereof.
Background
Abelmoschus manihot (L.) Medic, a dry corolla of Abelmoschus manihot (L.) Medic) belonging to family Malvaceae, is sweet and cold in taste and enters kidney and bladder meridians; has effects of clearing away heat and toxic materials, eliminating dampness, and relieving swelling, and can be used for treating superficial infection, toxic swelling, and scald caused by water and fire. The medicine is recorded in Jiayou materia Medica, and the Chinese pharmacopoeia of 2010 edition. Record of Jiayou herbal: abelmoschus manihot is mainly used for treating sore and pus which are not healed for a long time and is applied as powder. The compendium of materia Medica (Ben Cao gang mu) is characterized in that: abelmoschus manihot, flos Abelmoschi Manihot, with sweet, cold, slippery and non-toxic smell, is used as a key herb for treating sore when patients with malignant sores and pus are not healed for a long time.
According to the research results of published documents, the flavonoid compound is the main component of the flower of abelmoschus manihot and is also the pharmacological active component of the flower of abelmoschus manihot, and the flower of abelmoschus manihot total flavone can improve the renal function and has obvious curative effect on treating chronic glomerulonephritis. Modern researches prove that the flavonoid components in the abelmoschus manihot extract not only have obvious treatment effect on sores, but also have obvious protection effect on injuries of heart, brain, tissues and the like caused by ischemia; in addition, researches show that the sunset abelmoschus flower total flavone has certain effects on controlling intestinal inflammation, reducing histopathological scores and the like, wherein the kidney tissue inflammation factor level is reduced by dose group therapy in the sunset abelmoschus flower total flavone, and free radicals of organisms are eliminated at the same time, so that the sunset abelmoschus flower total flavone is expected to become a medicine for treating chronic glomerulonephritis. A plurality of literature reports show that the sunset abelmoschus flower total flavone has better effects on the aspects of resisting inflammation, relieving fever and pain, protecting heart and brain ischemia injury, promoting angiogenesis, reducing thrombus, reducing blood sugar, resisting virus, resisting depression and the like. In addition, in recent years, cosmetics of various countries in the world have been mainly developed in a direction of "chongshang nature", and natural plant materials have been favored. The flavonoid compounds are widely existed in the plant world, and many of the flavonoid compounds have the effects of removing free radicals in skin, promoting skin metabolism, reducing pigmentation, moistening skin, astringing and moisturizing, removing red blood streak and the like, but at present, cosmetics added with the plant flavonoid compounds are still in the research and development stage.
The extraction method of the flower of abelmoschus manihot reported in the literature comprises ethanol reflux extraction, ultrasonic extraction and normal-temperature soaking extraction, for example, Chinese patent application 201510916167.7 discloses an extraction process of flavonoid compounds in the flower of abelmoschus manihot, which comprises the following steps: drying flos Abelmoschi Manihot, pulverizing, sieving, adding ethanol, ultrasonic extracting, centrifuging, collecting supernatant, and filtering. For another example, chinese patent application 201911306130.7 discloses an extract of flower of abelmoschus manihot and a preparation method thereof, the preparation method comprising the steps of: (1) extraction: weighing raw material abelmoschus manihot, adding 60-80% ethanol for reflux extraction; (2) first filtration: filtering to obtain filtrate; (3) concentration: concentrating the filtrate under reduced pressure to obtain concentrated solution a without alcohol smell, and recovering ethanol; (4) water precipitation: adding water into the concentrated solution a for water precipitation; (5) and (3) second filtration: filtering to obtain supernatant; (6) adsorption: adsorbing the supernatant with macroporous resin; (7) impurity washing: washing impurities with water; (8) desorbing: desorbing by using 65-75% ethanol to obtain desorption solution; (9) concentration: concentrating the desorption solution under reduced pressure to obtain concentrated solution b, wherein the Baume degree is 10-20; (10) and (3) drying: and transferring the concentrated solution b to a spraying process for spraying to obtain the product. The Abelmoschus manihot flower extract has good hygroscopicity. The preparation process is safer, more efficient and more environment-friendly.
However, the sunset abelmoschus flower extract has complex components, the content of active ingredients is greatly changed, different content compositions generally have great influence on the pharmacological action of the sunset abelmoschus flower extract, but the actual research of the sunset abelmoschus flower extract in cosmetics is relatively deficient at present, the extraction transfer rate is low, the extraction energy consumption is high, and the solvent dosage is large. Therefore, there is a need to search for effective fractions of sunscreens for cosmetics, particularly for preventing or treating skin aging, or anti-aging cosmetics, and extraction processes thereof.
Disclosure of Invention
The invention aims to provide an effective part of flavones of abelmoschus manihot and a preparation method and application thereof, and provides the effective part of flavones of abelmoschus manihot and an extraction process thereof aiming at cosmetics, in particular sunscreens, after-sun repairing agents or anti-aging cosmetics for preventing or treating skin aging.
In order to achieve the purpose, the technical scheme of the invention is as follows:
firstly, the invention provides an effective part of flavones of abelmoschus manihot, which comprises the following flavones: quercetin, quercetin-3' -O-glucoside, myricetin, gossypetin-8-O-beta-D-glucuronide, isoquercitrin, rutin and hyperin, wherein the mass ratio of the components is 1:13-33:1-7:14-38:12-32:1-5:18-42, preferably 1:15-32:2-6:16-36:14-30:2-4: 20-40; preferably 1:17-29:2.4-5.2:18-33:16-27:2.4-3.6: 23-38; further preferably 1:19-26:2.7-4.4:20-29:18-24:2.7-3.3: 26-35.
Preferably, in the effective part, the content of quercetin, quercetin-3' -O-glucoside, myricetin, gossypetin-8-O-beta-D-glucuronide, isoquercitrin, rutin and hyperoside is 52% or more, preferably 56% or more, more preferably 63-77%, and still more preferably 67-75%. Furthermore, the invention provides a pharmaceutical composition comprising the effective part, and the pharmaceutical composition further comprises a pharmaceutically acceptable carrier.
Preferably, the dosage form of the pharmaceutical composition comprises solution, injection, tablet, suppository, ointment, gel, pill, granule, capsule, mixture and suspension.
Furthermore, the invention provides a composition comprising the following flavonoid ingredients: quercetin, quercetin-3' -O-glucoside, myricetin, gossypetin-8-O-beta-D-glucuronide, isoquercitrin, rutin and hyperoside, wherein the mass ratio of the components is 1:13-33:1-7:14-38:12-32:1-5:18-42, preferably 1:15-32:2-6:16-36:14-30:2-4:20-40, more preferably 1:17-29:2.4-5.2:18-33:16-27:2.4-3.6:23-38, and even more preferably 1:19-26:2.7-4.4:20-29:18-24:2.7-3.3: 26-35.
Preferably, in the composition, the content of quercetin, quercetin-3' -O-glucoside, myricetin, gossypetin-8-O-beta-D-glucuronide, isoquercitrin, rutin and hyperoside is 52% or more, preferably 56% or more, more preferably 63-77%, and still more preferably 67-75%.
Furthermore, the invention provides the application of the effective part, the pharmaceutical composition or the composition in preparing a sun-screening agent, a post-basking repairing agent or an anti-aging cosmetic for preventing or treating skin aging.
Furthermore, the invention provides application of the effective part, the pharmaceutical composition or the composition in preparing anti-aging drugs.
Furthermore, the invention provides a preparation method of the effective part, and particularly provides a method for preparing high-purity flavone components of the abelmoschus manihot by a membrane separation coupling resin method. The method comprises the steps of gradually separating total flavonoids from the flower of abelmoschus manihot by using an ultrafiltration membrane and macroporous resin, extracting the flower of abelmoschus manihot by using ethanol, primarily treating an extracting solution, filtering by using ultrafiltration membranes with different molecular weight cut-off to obtain a concentrated solution, recovering the ethanol from the concentrated solution, and treating by using the macroporous resin to obtain the high-purity effective flavonoid fraction of the flower of abelmoschus manihot.
The preparation method comprises the following steps:
(1) extracting flos Abelmoschi Manihot with ethanol to obtain extractive solution; (2) the extract is filtered in series by two ultrafiltration membranes with different cut-off molecular weights to prepare a cut-off concentrated solution; (3) removing ethanol from the concentrated solution, and eluting with macroporous resin to obtain effective fraction of flos Abelmoschi Manihot flower flavonoids.
Preferably, the first and second liquid crystal materials are,
in the step (1), the dosage of the ethanol is 10-25 times of that of the flower of abelmoschus manihot, the ethanol is 60% -95% ethanol solution, and the extraction method can adopt the extraction method used in the field, including but not limited to a reflux method or a percolation method;
in the step (2), the molecular weight is 300-; the filtering volume of the filtration is 50-90% of the extracting solution, and the preferred filtering volume is 70-80%;
in the step (2), before filtering, the method further comprises the steps of extracting the extracting solution, adsorbing with activated carbon, precipitating with alcohol or precipitating with acid, wherein the solvent for precipitating with alcohol is preferably ethanol or methanol, and the solvent for precipitating with acid is preferably hydrochloric acid or sulfuric acid.
In the step (3), the model of the macroporous resin is D101, HPD100 or AB-8, and the ethanol removal is the decompression recovery of ethanol at the temperature of 50-90 ℃;
in the step (3), the elution process of the macroporous resin comprises the following steps: the diameter-height ratio of the macroporous resin is 1:6, the concentration of a sample loading solution is 0.15g crude drug/ml, the volume of the sample loading solution is 7BV, sample loading is carried out at the flow rate of 2BV/h, impurities are removed by using 6BV pure water and 3BV 5% ethanol at the flow rate of 2BV/h, and elution is carried out by using 4BV 60% ethanol at the flow rate of 2 BV/h. The sample loading liquid takes water as a solvent.
Further preferably, the preparation method provided by the invention comprises the following specific operation steps:
(1) extracting Abelmoschus manihot with 10-25 times of 60% -95% ethanol to obtain Abelmoschus manihot extract;
(2) primarily treating the abelmoschus manihot extract, and filtering with ultrafiltration membranes with different molecular weight cut-off, wherein the primary treatment method comprises extraction, activated carbon adsorption, alcohol precipitation or acid precipitation and the like;
(3) selecting ultrafiltration membranes with cut-off molecular weight of 500-3500, using the ultrafiltration membranes with different molecular weights in series, filtering 50-90% of the volume of the extract by using the ultrafiltration membranes to obtain concentrated solution, recovering ethanol from the concentrated solution at 50-90 ℃ under reduced pressure, and treating the ethanol by using macroporous resin to obtain the flavonoid effective part of the flower of abelmoschus manihot, wherein the type of the macroporous resin 1:6 is D101, HPD100 or Ab-8;
(4) the treatment process of the macroporous resin comprises the following steps: the diameter-height ratio of the macroporous resin is 1:4-1:9, the concentration of a sample loading solution is 0.10-0.30g crude drug/ml, the volume of the sample loading solution is 4-12BV, sample loading is carried out at the flow rate of 1-4BV/h, impurity removal is carried out by using 4-8BV pure water and 1-5BV 5% ethanol at the flow rate of 0.5-4BV/h, and elution is carried out by using 2-8BV 60% ethanol at the flow rate of 1-5 BV/h;
(5) recovering ethanol from macroporous resin eluate at 50-90 deg.C under reduced pressure to obtain flos Abelmoschi Manihot flavone effective fraction.
Still more preferably as follows:
(1) extracting Abelmoschus manihot with 15-18 times of 60% -70% ethanol to obtain Abelmoschus manihot extract;
(2) primarily treating the abelmoschus manihot extract, and filtering with ultrafiltration membranes with different molecular weight cut-off, wherein the primary treatment method comprises extraction, activated carbon adsorption, alcohol precipitation or acid precipitation and the like;
(3) selecting ultrafiltration membranes with the cut-off molecular weight of 500-3500, connecting the ultrafiltration membranes with different molecular weights in series for use, filtering 70-90% of the volume of an extracting solution by using the ultrafiltration membranes to obtain a concentrated solution, recovering ethanol from the concentrated solution at 50-70 ℃ under reduced pressure, and treating the concentrated solution by using D101 macroporous resin to obtain the flavonoid effective part of the flower of abelmoschus manihot;
(4) the treatment process of the macroporous resin comprises the following steps: the diameter-height ratio of the macroporous resin is 1:5-1:8, the concentration of a sample loading solution is 0.10-0.20g crude drug/ml, the volume of the sample loading solution is 5-10BV, sample loading is carried out at the flow rate of 1-3BV/h, impurity removal is carried out by 5-7BV pure water and 2-4BV 5% ethanol at the flow rate of 1-3BV/h, and elution is carried out by 3-6BV 60% ethanol at the flow rate of 1-4 BV/h;
(5) recovering ethanol from macroporous resin eluate at 50-70 deg.C under reduced pressure to obtain flos Abelmoschi Manihot flavone effective fraction.
The invention has the beneficial effects that:
(1) the flavonoid effective part of the abelmoschus manihot has good effects of preventing or treating sun screening and repairing after solarization;
(2) the flavonoid effective part of the abelmoschus manihot has good anti-aging effect;
(3) the preparation method has the advantages of simple process, short production period, mild treatment conditions, low energy consumption, good separation effect of the 7 flavonoid components of the flower of abelmoschus manihot, wide sources of the used raw materials and reagents, low cost and easy realization of industrial large-scale production.
Detailed Description
The present invention will be further explained with reference to specific examples in order to make the technical means, the technical features, the technical objectives and the effects of the present invention easier to understand, but the following examples are only preferred embodiments of the present invention, and not all embodiments of the present invention. Based on the embodiments in the implementation, other embodiments obtained by those skilled in the art without any creative efforts belong to the protection scope of the present invention. In the following examples, unless otherwise specified, all the procedures and equipment used were conventional procedures and equipment used was conventional equipment.
Example 1 preparation of effective fractions of sunset abelmoschus flowers
Pulverizing 100g flos Abelmoschi Manihot into coarse powder, and extracting with 15 times of 60% ethanol under reflux to obtain extractive solution; adsorbing the abelmoschus manihot extract by using activated carbon, filtering by using an ultrafiltration membrane with the molecular weight cutoff of 3500, collecting filtrate, filtering 80% of the filtrate by using an ultrafiltration membrane with the molecular weight cutoff of 500 to obtain concentrated solution, recovering ethanol from the concentrated solution at 50 ℃ under reduced pressure, and treating by using D101 macroporous resin, wherein the treatment process of the macroporous resin comprises the following steps: the diameter-height ratio of the macroporous resin is 1:6, the concentration of a sample loading solution (aqueous solution) is 0.15g crude drug/ml, the volume of the sample loading solution is 7BV, sample loading is carried out at the flow rate of 2BV/h, impurities are successively removed by 6BV pure water and 3BV 5% ethanol at the flow rate of 2BV/h, elution is carried out by 4BV 60% ethanol at the flow rate of 2BV/h to obtain an eluent, and the eluent is decompressed and recycled at the temperature of 50 ℃ to obtain 1.23g of the effective part of the flower flavonoid of abelmoschus manihot.
Example 2 preparation of effective fractions of sunset abelmoschus flowers
Pulverizing 100g flos Abelmoschi Manihot into coarse powder, and extracting with 18 times of 70% ethanol under reflux to obtain extractive solution; filtering the abelmoschus manihot extract by using an ultrafiltration membrane with molecular weight cutoff of 3500, collecting filtrate, filtering 70% of the filtrate by using an ultrafiltration membrane with molecular weight cutoff of 1000 to obtain concentrated solution, recovering ethanol from the concentrated solution at 60 ℃ under reduced pressure, and treating the concentrated solution by using D101 macroporous resin, wherein the treatment process of the macroporous resin comprises the following steps: the diameter-height ratio of the macroporous resin is 1:5, the concentration of a sample loading solution is 0.15g crude drug/ml, the volume of the sample loading solution is 6BV, sample loading is carried out at the flow rate of 2BV/h, impurities are removed by 6BV pure water and 3BV 5% ethanol at the flow rate of 2BV/h, elution is carried out by 4BV 60% ethanol at the flow rate of 1.5BV/h to obtain an eluent, and the eluent is decompressed and recycled at the temperature of 60 ℃ to obtain 1.19g of the effective part of the abelmoschus manihot flavonoids.
Example 3 preparation of effective fractions of sunset abelmoschus flowers
Pulverizing 100g flos Abelmoschi Manihot into coarse powder, percolating with 18 times of 60% ethanol, and extracting to obtain extractive solution; filtering the abelmoschus manihot extract by using an ultrafiltration membrane with molecular weight cutoff of 3500, collecting filtrate, filtering 80% of the filtrate by using an ultrafiltration membrane with molecular weight cutoff of 500 to obtain concentrated solution, recovering ethanol from the concentrated solution at 60 ℃ under reduced pressure, and treating the concentrated solution by using D101 macroporous resin, wherein the treatment process of the macroporous resin comprises the following steps: the diameter-height ratio of the macroporous resin is 1:8, the concentration of a sample loading solution is 0.15g crude drug/ml, the volume of the sample loading solution is 8BV, sample loading is carried out at the flow rate of 2BV/h, impurities are removed by using 6BV pure water and 3BV 5% ethanol at the flow rate of 2BV/h, elution is carried out by using 4BV 60% ethanol at the flow rate of 3BV/h to obtain an eluent, and the eluent is decompressed at the temperature of 60 ℃ to recover the ethanol to obtain 0.98g of the effective part of the flower flavonoid of abelmoschus manihot.
Example 4 preparation of effective fractions of sunset abelmoschus flowers
Percolating 100g flos Abelmoschi Manihot with 18 times of 70% ethanol to obtain extractive solution; filtering the abelmoschus manihot extract by using an ultrafiltration membrane with molecular weight cutoff of 3500, collecting filtrate, filtering 80% of the filtrate by using an ultrafiltration membrane with molecular weight cutoff of 1000, washing the liquid in a charging basket by using 70% ethanol, washing 3 times of the volume of the liquid to obtain concentrated solution, recovering ethanol from the concentrated solution at 60 ℃ under reduced pressure, and treating the concentrated solution by using D101 macroporous resin, wherein the treatment process of the macroporous resin comprises the following steps: the ratio of diameter to height of the macroporous resin is 1:6, the concentration of a sample loading solution is 0.15g crude drug/ml, the volume of the sample loading solution is 7BV, sample loading is carried out at the flow rate of 2BV/h, impurities are removed by using 6BV pure water and 3BV 5% ethanol at the flow rate of 2BV/h, elution is carried out by using 4BV 60% ethanol at the flow rate of 2BV/h to obtain an eluent, and the eluent is decompressed and recycled at the temperature of 60 ℃ to obtain 1.25g of the effective part of the flower flavonoid of abelmoschus manihot.
Example 5 detection of effective fractions of sunset abelmoschus flowers
The content of 7 ingredients was measured on the effective fractions of sunset abelmoschus flower flavonoid prepared in examples 1 to 4. The detection method adopts a UPLC method reported in 7 ingredients in Abelmoschus manihot (journal of drug analysis, 12 th stage 2013, 2082-2087) for determining the content of the ingredients in Abelmoschus manihot by a one-test-multiple evaluation method.
The detection results of the components in the sample are shown in tables 1 to 4:
TABLE 1 assay data for the sample of example 1
TABLE 2 assay data for the sample of example 2
TABLE 3 assay data for the samples of example 3
TABLE 4 assay data for the samples of example 4
Example 6 prevention of UVB-induced skin Damage in mice by effective fractions of Abelmoschus manihot flavonoid
The experimental method comprises the following steps:
BALB/c mice, weight 22 + -2 g, light/dark cycle 12 h. When UVB irradiates, a 313nm UVB lamp tube 4 is used for manufacturing an ultraviolet lamp box, the irradiation height is adjusted to be 20cm, 2 hours of irradiation are carried out every day, and the irradiation lasts for four weeks.
Randomly dividing the test result into a control group, a light aging model group, an abelmoschus manihot flavonoid effective part prevention group, an abelmoschus manihot flavonoid effective part treatment group and an abelmoschus manihot extract control group according to the weight, wherein each group comprises 6 patients. Wherein the effective part of the flower flavonoid of abelmoschus manihot is prepared according to the preparation method of the embodiment 3, and the flower extract of abelmoschus manihot is prepared according to the embodiment 3 of the document CN 108567802A. After grouping, the back of each group of mice is depilated until the skin is completely exposed, and the depilated area is 6-8cm2。
Control group, without UVB irradiation, was directly applied with physiological saline (0.1 mL/cm)2) (ii) a A light aging model group, wherein the back of the mouse after depilation is irradiated by a UVB lamp; the effective part prevention group of flos Abelmoschi Manihot flavone is prepared by smearing effective part solution of flos Abelmoschi Manihot flavone (active ingredient: 0.05 mg/cm) 1 hr before each UVB irradiation2) (ii) a The flos Abelmoschi Manihot flavone effective part treatment group is smeared with flos Abelmoschi Manihot flavone effective part solution (active ingredient 0.05 mg/cm) 1 hr after each UVB irradiation2) (ii) a The flos Abelmoschi Manihot extract treatment group is applied with flos Abelmoschi Manihot extract solution (active ingredient 0.15 mg/cm) 1 hr after each UVB irradiation2)。
After the experiment is finished, the skin of the back of each group of mice is photographed by a digital camera, and the damage degree of the skin of the back of the mice is observed and analyzed.
The results of the experiment are shown in table 5:
table 5.
The experimental result shows that the effective part of the flavone of the abelmoschus manihot can effectively prevent or treat skin damage caused by ultraviolet irradiation, and can play a role in sun protection, repair and aging resistance.
The present invention is not limited to the above-described preferred embodiments, but rather, the present invention is to be construed broadly and cover all modifications, equivalents, and improvements falling within the spirit and scope of the present invention.
Claims (10)
1. The effective part of the flavones of the flower of abelmoschus manihot is characterized by comprising the following flavones: quercetin, quercetin-3' -O-glucoside, myricetin, gossypetin-8-O-beta-D-glucuronide, isoquercitrin, rutin and hyperin, wherein the mass ratio of the components is 1:13-33:1-7:14-38:12-32:1-5: 18-42.
2. The effective part according to claim 1, characterized by comprising the following flavonoid ingredients: quercetin, quercetin-3' -O-glucoside, myricetin, gossypetin-8-O-beta-D-glucuronide, isoquercitrin, rutin and hyperin, wherein the mass ratio of the components is 1:15-32:2-6:16-36:14-30:2-4: 20-40; preferably 1:17-29:2.4-5.2:18-33:16-27:2.4-3.6: 23-38; further preferably 1:19-26:2.7-4.4:20-29:18-24:2.7-3.3: 26-35.
3. The effective component according to claim 1, wherein the content of quercetin, quercetin-3' -O-glucoside, myricetin, gossypetin-8-O- β -D-glucuronide, isoquercitrin, rutin and hyperoside is 52% or more, preferably 56% or more, more preferably 63-77%, still more preferably 67-75%.
4. A pharmaceutical composition comprising the effective site of any one of claims 1 to 3, wherein the pharmaceutical composition further comprises a pharmaceutically acceptable carrier.
5. The pharmaceutical composition according to claim 4, wherein the pharmaceutical composition is in the form of solution, injection, tablet, suppository, ointment, gel, pill, granule, capsule, mixture, and suspension.
6. A composition characterized by comprising the following flavonoid ingredients: quercetin, quercetin-3' -O-glucoside, myricetin, gossypetin-8-O-beta-D-glucuronide, isoquercitrin, rutin and hyperoside, wherein the mass ratio of the components is 1:13-33:1-7:14-38:12-32:1-5:18-42, preferably 1:15-32:2-6:16-36:14-30:2-4:20-40, more preferably 1:17-29:2.4-5.2:18-33:16-27:2.4-3.6:23-38, and even more preferably 1:19-26:2.7-4.4:20-29:18-24:2.7-3.3: 26-35.
7. Use of the active site according to any one of claims 1 to 3, the pharmaceutical composition according to claim 4 or 5, or the composition according to claim 6 for the preparation of a sunscreen, a post-sun repair agent, or an anti-aging cosmetic for preventing or treating skin aging.
8. Use of the active site of any one of claims 1-3, the pharmaceutical composition of claim 4 or 5, or the composition of claim 6 for the manufacture of an anti-aging medicament.
9. The method for producing the effective fraction according to any one of claims 1 to 3, characterized by comprising the steps of: (1) extracting flos Abelmoschi Manihot with ethanol to obtain extractive solution; (2) filtering the extracting solution by using ultrafiltration membranes with two different cut-off molecular weights to prepare a concentrated solution; (3) removing ethanol from the concentrated solution, and eluting with macroporous resin to obtain effective components of flos Abelmoschi Manihot flower flavonoids.
10. The method according to claim 9, wherein the ethanol in step (1) is 10-25 times the amount of the flower of abelmoschus manihot, and the ethanol is 60% -95% ethanol solution; in the step (2), the molecular weight is 300-3500, preferably the two molecular weight cutoffs are 500 and 3500 respectively, and the filtered volume of the filtration is 50-90 percent of the extracting solution, preferably 70-80 percent; in the step (2), preferably before filtering, the method further comprises the steps of extracting the extracting solution, adsorbing by activated carbon, precipitating by alcohol or precipitating by acid; the model of the macroporous resin in the step (3) is D101, HPD100 or AB-8, and the elution process of the macroporous resin comprises the following steps: the diameter-height ratio of the macroporous resin is 1:4-1:9, the concentration of a sample loading solution is 0.10-0.30g crude drug/ml, the volume of the sample loading solution is 4-12BV, sample loading is carried out at the flow rate of 1-4BV/h, impurity removal is carried out by using 4-8BV pure water and 1-5BV 5% ethanol at the flow rate of 0.5-4BV/h, and elution is carried out by using 2-8BV 60% ethanol at the flow rate of 1-5 BV/h.
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