CN107823260A - A kind of compound skin cream for treating chloasma, preparation method and application - Google Patents

A kind of compound skin cream for treating chloasma, preparation method and application Download PDF

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Publication number
CN107823260A
CN107823260A CN201711158919.3A CN201711158919A CN107823260A CN 107823260 A CN107823260 A CN 107823260A CN 201711158919 A CN201711158919 A CN 201711158919A CN 107823260 A CN107823260 A CN 107823260A
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parts
medicinal extract
preparation
skin cream
chloasma
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蔡瑞康
戴博
张华峰
袁海龙
吴燕
沈成英
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/25Araliaceae (Ginseng family), e.g. ivy, aralia, schefflera or tetrapanax
    • A61K36/258Panax (ginseng)
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/28Asteraceae or Compositae (Aster or Sunflower family), e.g. chamomile, feverfew, yarrow or echinacea
    • A61K36/286Carthamus (distaff thistle)
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/57Magnoliaceae (Magnolia family)
    • A61K36/575Magnolia
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/44Oils, fats or waxes according to two or more groups of A61K47/02-A61K47/42; Natural or modified natural oils, fats or waxes, e.g. castor oil, polyethoxylated castor oil, montan wax, lignite, shellac, rosin, beeswax or lanolin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/0012Galenical forms characterised by the site of application
    • A61K9/0014Skin, i.e. galenical aspects of topical compositions
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/06Ointments; Bases therefor; Other semi-solid forms, e.g. creams, sticks, gels
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/30Extraction of the material
    • A61K2236/33Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/331Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/30Extraction of the material
    • A61K2236/33Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/333Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/30Extraction of the material
    • A61K2236/39Complex extraction schemes, e.g. fractionation or repeated extraction steps
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/51Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/53Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization

Abstract

A kind of compound skin cream for treating chloasma of the present invention, belongs to traditional Chinese medicine external used medicine technical field.Preparation method includes:The emulsification product of the preparation of pseudo-ginseng medicinal extract, safflower medicinal extract and flower bud of lily magnolia medicinal extract, the preparation of oil phase, the preparation of aqueous phase, the emulsification of oil phase and aqueous phase, oil phase and aqueous phase adds pseudo-ginseng medicinal extract, safflower medicinal extract and flower bud of lily magnolia medicinal extract, and temperature is down to 55 DEG C, adds ginger extrait;Temperature is down to 37 DEG C of dischargings, produces.The compound skin cream of gained is prepared by the above method.Compound skin cream is preparing the application in treating chloasma medicine.The present invention has advantages below:To the direct smearing in affected part, mitigate pain during patient's treatment;With promoting blood circulation, wind-dispelling, stagnant, the lustrous and transparent flesh of row effect pseudo-ginseng medicinal extract, safflower medicinal extract, flower bud of lily magnolia medicinal extract, the compound preparation has preferable therapeutic effect.

Description

A kind of compound skin cream for treating chloasma, preparation method and application
Technical field
The invention belongs to traditional Chinese medicine external used medicine technical field, and in particular to a kind of compound skin breast for treating chloasma Paste, preparation method and application.
Background technology
Chloasma is a kind of common skin pigment dysbolism disease, is apt to occur in Female in child bearing period, but each age, kind Race, the colour of skin, men and women can fall ill.Chloasma is apt to occur in cheek, lip week, forehead, accidental to be answered in upper limbs, its cause of disease and pathogenesis It is miscellaneous, although chloasma is not unhealthful, occurs in facial exposure portion, have a strong impact on attractive in appearance, easily cause essence to patient On god or psychological pain.It is indefinite due to the cause of disease, easily examine refractory, be a big difficult disease of current dermatological field Disease.
Now, the method for treating chloasma mainly has:For oral administration, external used medicine, laser or Photon Thherapy, kinds of schemes joint Treatment etc..Although most for the treatment of methods can make the patient's condition have some improvement, because the chloasma cause of disease is imperfectly understood, stop Easily recurred after medicine.
The content of the invention
It is an object of the invention to disclose a kind of compound skin cream for treating chloasma.
Second object of the present invention is to disclose a kind of preparation side for the compound skin cream for treating chloasma Method.
Third object of the present invention is the application for disclosing the compound skin cream of above-mentioned treatment chloasma.
The purpose of the present invention is achieved through the following technical solutions:
A kind of compound skin cream for treating chloasma, wherein, the compound skin cream is by following weight The raw material of part is made:0.25 part of 2.4 parts of pseudo-ginseng, 0.2 part of the flower bud of lily magnolia, 0.14 part of safflower, oil phase, aqueous phase and ginger extrait;
The oil phase is made from the following raw materials in parts by weight:1.5 parts of dimeticones, 2 parts of Ak6,1 part of Ak25, octadecyl alcolol 4 Part, 2 parts of single, double tristerin, 1 part of beeswax, 0.8 part of stearic acid, 8 parts of light liquid petrolatum.
The aqueous phase is made from the following raw materials in parts by weight:12 parts of glycerine, 0.25 part of ethyl hydroxy benzoate and purified water 65.83 Part.
A kind of preparation method for being used to treat the compound skin cream of chloasma, comprises the steps:
(1), the preparation of pseudo-ginseng medicinal extract:2.4 parts of pseudo-ginseng is taken, soaks 2h, then boils and carries 2 times, the 1st time plus 8 times of water Amount, decocts 1.5h, the 2nd time plus 6 times of water amount, decocts 1h, extract solution filtration, merging filtrate, be concentrated under reduced pressure into about per ml equivalent to 1g medicinal materials, lower 2 times of amount ethanol of addition are stirred, 48h is refrigerated, separates supernatant, reclaim ethanol and be concentrated into every g medicinal extract and contain 2g medicines The medicinal extract of material, pseudo-ginseng medicinal extract is produced, it is standby;
(2), the preparation of safflower medicinal extract:0.14 part of safflower is taken, soaks 2h, then boils and carries 2 times, the 1st time plus 8 times of water Amount, decocts 1.5h, the 2nd time plus 6 times of water amount, decocts 1h, extract solution filtration, merging filtrate, be concentrated under reduced pressure into about per ml equivalent to 1g medicinal materials, lower 2 times of amount ethanol of addition are stirred, 48h is refrigerated, separates supernatant, reclaim ethanol and be concentrated into every g medicinal extract and contain 2g medicines The medicinal extract of material, safflower medicinal extract is produced, it is standby;
(3), the preparation of flower bud of lily magnolia medicinal extract:Take 0.2 part of the flower bud of lily magnolia, add 70% ethanol soak 1h, be then refluxed for extraction 2 times, the 1st Secondary plus 8 times of amounts of alcohol, flow back 1.5h, and the 2nd time plus 6 times of amounts of alcohol, flow back 1h, extract solution filtration, merging filtrate, ethanol is recovered under reduced pressure, And the medicinal extract that every g medicinal extract contains 2g medicinal materials, as flower bud of lily magnolia medicinal extract are concentrated into, it is standby;
(4), the preparation of oil phase:Raw material, 1.5 parts of dimeticones, 2 parts of Ak6,1 part of Ak25,18 are weighed by following parts by weight 4 parts of alcohol, 2 parts of single, double tristerin, 1 part of beeswax, 0.8 part of stearic acid, 8 parts of light liquid petrolatum;By octadecyl alcolol, beeswax, Light liquid petrolatum, dimeticone, Ak25, Ak6, stearic acid and single, double tristerin, put into oil cauldron, 80-85 DEG C of water-bath Heating is molten into oil phase, and 80-85 DEG C of insulation is standby;
(5), the preparation of aqueous phase:Raw material, 12 parts of glycerine, 0.25 part of ethyl hydroxy benzoate, purified water are weighed by following parts by weight 65.83 parts;It is aqueous phase that glycerine, purified water, which are dissolved by heating, when being heated to 60 DEG C, spreads addition ethyl hydroxy benzoate slowly;
(6), emulsify:The oil phase and heated aqueous of step (4) and (5) preparation gained are simultaneously stirred to 80-85 DEG C, and main cooker heats To 50-60 DEG C, oil phase is first pumped into main cooker by aqueous phase suction main cooker and after crossing 120 mesh sieves and crosses 120 mesh sieves, opens and stirs 35.0HZ, emulsify frequency 50.0HZ, emulsification times 20 minutes;
(7), main cooker is heated to the product for adding step (1), step (2) and step (3) after 60 DEG C, emulsifies frequency 50.0HZ, Emulsification times 20 minutes;Insulated and stirred frequency 35.0HZ, mixing time 20 minutes;At equal temperature, high pressure homogenizer is transferred to In, 3 circles are circulated under 10000psi newborn even pressure, are taken out, lead to cooling water temperature, temperature is down to less than 50 DEG C, stirring frequency For 30.0HZ;
(8), temperature is down to 55 DEG C, adds the ginger extrait that parts by weight are 0.25 part;Temperature is down to 37 DEG C of dischargings, i.e., handy In the compound skin cream for the treatment of chloasma.
A kind of compound skin cream for being used to treat chloasma, wherein, the compound skin cream is by above-mentioned Preparation method described in technical scheme prepares gained.
A kind of compound skin cream for treating chloasma described in above-mentioned technical proposal is yellowish-brown in preparation treatment Application in spot medicine.
The formulation of product of the present invention is cream, and character is white uniformity cream, and application method is applied to be only for external application Affected part, inspection, loading amount, granularity and limit test of microbe meet《Chinese Pharmacopoeia》Under the two annex cream items of version in 2015 Pertinent regulations.
The invention has the advantages that:
1st, this product uses cream form, to the direct smearing in affected part, during chloasma is treated, mitigates patient's treatment When pain.
2nd, present invention employs share with promoting blood circulation, wind-dispelling, capable stagnant, lustrous and transparent flesh effect pseudo-ginseng medicinal extract, safflower medicinal extract, the flower bud of lily magnolia Medicinal extract, the compound preparation have preferable therapeutic effect;Product of the present invention has carried out control by experiment, to its skin to its quality Skin excitant and clinical efficacy have carried out Primary Study.
Brief description of the drawings:
1st, Fig. 1 is indentification by TLC pseudo-ginseng result figure, and wherein row 1 are pseudo-ginseng control medicinal material, and row 2 are sample, and row 3 are Sample, row 4 are sample, and row 5 are negative control.
2nd, Fig. 2 is that reference substance solution HPLC schemes in test example 2.
3rd, Fig. 3 is that need testing solution HPLC schemes in test example 2.
4th, Fig. 4 is that negative control solution HPLC schemes in test example 2.
Embodiment:
To readily appreciate technical scheme, chloasma is treated to one kind of the present invention below in conjunction with specific test example Compound skin cream and preparation method thereof be further described.
Embodiment 1:A kind of preparation method for being used to treat the compound skin cream of chloasma, comprises the steps:
(1), the preparation of pseudo-ginseng medicinal extract:Pseudo-ginseng 24g is taken, soaks 2h, then boils and carries 2 times, the 1st time plus 8 times of amounts of water, is decocted 1.5h is boiled, the 2nd time plus 6 times of amounts of water, 1h is decocted, extract solution filtration, merging filtrate, is concentrated under reduced pressure into about per ml equivalent to 1g medicines Material, lower 2 times of amount ethanol of addition are stirred, 48h is refrigerated, separates supernatant, reclaim ethanol and be concentrated into every g medicinal extract and contain 2g medicinal materials Medicinal extract, pseudo-ginseng medicinal extract is produced, it is standby;
(2), the preparation of safflower medicinal extract:Safflower 1.4g is taken, soaks 2h, then boils and carries 2 times, the 1st time plus 8 times of amounts of water, 1.5h is decocted, the 2nd time plus 6 times of amounts of water, 1h is decocted, extract solution filtration, merging filtrate, is concentrated under reduced pressure into about per ml equivalent to 1g medicines Material, lower 2 times of amount ethanol of addition are stirred, 48h is refrigerated, separates supernatant, reclaim ethanol and be concentrated into every g medicinal extract and contain 2g medicinal materials Medicinal extract, safflower medicinal extract is produced, it is standby;
(3), the preparation of flower bud of lily magnolia medicinal extract:Take flower bud of lily magnolia 2g, add 70% ethanol soak 1h, be then refluxed for extraction 2 times, the 1st time plus 8 times of amounts of alcohol, flow back 1.5h, and the 2nd time plus 6 times of amounts of alcohol, flow back 1h, extract solution filtration, merging filtrate, ethanol is recovered under reduced pressure, and dense The medicinal extract that every g medicinal extract contains 2g medicinal materials, as flower bud of lily magnolia medicinal extract are reduced to, it is standby;
(4), the preparation of oil phase:Raw material, 15g dimeticones, 20g Ak6,10g Ak25,18 are weighed by following parts by weight Alcohol 40g, single, double tristerin 20g, beeswax 10g, stearic acid 8g, light liquid petrolatum 80g;By octadecyl alcolol, beeswax, light Matter liquid paraffin, dimeticone, Ak25, Ak6, stearic acid and single, double tristerin, put into oil cauldron, and 80-85 DEG C of water-bath adds Hot melt turns to oil phase, and 80-85 DEG C of insulation is standby;
(5), the preparation of aqueous phase:Raw material, glycerine 120g, ethyl hydroxy benzoate 2.5g, purified water are weighed by following parts by weight 658.3g;It is aqueous phase that glycerine, purified water, which are dissolved by heating, when being heated to 60 DEG C, spreads addition ethyl hydroxy benzoate slowly;
(6), emulsify:The oil phase and heated aqueous of step (4) and (5) preparation gained are simultaneously stirred to 80-85 DEG C, and main cooker heats To 50-60 DEG C, oil phase is first pumped into main cooker by aqueous phase suction main cooker and after crossing 120 mesh sieves and crosses 120 mesh sieves, opens and stirs 35.0HZ, emulsify frequency 50.0HZ, emulsification times 20 minutes;
(7), main cooker is heated to the product for adding step (1), step (2) and step (3) after 60 DEG C, emulsifies frequency 50.0HZ, Emulsification times 20 minutes;Insulated and stirred frequency 35.0HZ, mixing time 20 minutes;At equal temperature, high pressure homogenizer is transferred to In, 3 circles are circulated under 10000psi newborn even pressure, are taken out, lead to cooling water temperature, temperature is down to less than 50 DEG C, stirring frequency For 30.0HZ;
(8), temperature is down to 55 DEG C, adds the ginger extrait that parts by weight are 2.5g;Temperature is down to 37 DEG C of dischargings, produces and is used for Treat the compound skin cream of chloasma.
External application affected part, 1 time every night.
Below by way of specific test example to a kind of compound skin for treating chloasma of the present invention with cream (hereinafter referred to as:Dispel Spot frost) and preparation method thereof possessed by beneficial effect be further described.
Test example 1:Indentification by TLC pseudo-ginseng:
This product (preparing the product of gained according to the method for embodiment 1) 20g is taken, adds ethanol 40ml, stirs, filter, Filtrate 40ml is taken, water-bath is evaporated to about 10ml, adds water 10ml, lets cool, and adds petroleum ether 2 times, each 20ml, discards petroleum ether Liquid, then add chloroform to wash 2 times, each 20ml, chloroform liquid is discarded, aqueous adds n-butanol, and shaking is extracted twice, every time 20ml, merges and n-butanol liquid, ammonification test solution wash twice, and each 15ml, discards ammonia solution, n-butanol liquid is put to be steamed in water-bath Dry, residue adds methanol 1ml to make dissolving, as need testing solution.
Pseudo-ginseng control medicinal material 0.5g separately is taken, adds methanol 20ml, is ultrasonically treated 20 minutes, filtration, filtrate is evaporated, and residue adds first Alcohol 1ml makes dissolving, as control medicinal material solution.
According to thin-layered chromatography (《Chinese Pharmacopoeia》2015 editions four general rules 0502) experiment, absorption above two solution each 5~ 10 μ 1, put respectively on same silica gel g thin-layer plate, with n-butanol-ethyl acetate-water (4:1:5) upper solution is solvent, Expansion, take out, dry, spray with 10% ethanol solution of sulfuric acid, it is clear that hot blast is blown to spot development.In test sample chromatogram, with it is right According on the corresponding position of medicinal material chromatogram, show the spot of same color.
As a result as shown in figure 1, in wherein Fig. 1 row 1 be pseudo-ginseng control medicinal material, 2~row of row 4 be three batches of samples, row 5 are scarce The negative solution of pseudo-ginseng medicinal extract.
Test example 2:Determine ginsenoside Rb1's content in content in freckle cream:
1st, instrument and equipment and reagent:
Shimadzu 15C high performance liquid chromatographs (Japanese Shimadzu), TB-215D electronic balances (Denver's instrument (Beijing) limited public affairs Department), KQ-200DB type data ultrasonic cleaners (Kunshan Ultrasonic Instruments Co., Ltd.), six hole biserial water-baths (upper sea light Learn instrument plant), SHB-III multiplex vavuum pump of circulating water type (Zhengzhou Heng Yan Instrument Ltd.).
Ginsenoside Rb1(Nat'l Pharmaceutical & Biological Products Control Institute, lot number:110704-201424, purity:93.7%), second Nitrile (chromatographically pure, lot number 015900, MREDA), water (Wahaha Pure Water), methanol (analyze pure, lot number 20150621, Beijing Factory), content in freckle cream (preparation of the method for embodiment 1).
2nd, the selection of chromatographic condition:
Using《Chinese Pharmacopoeia》Mobile phase condition is tested under version psoralea corylifolia assay items in 2015, is ensureing to separate In the case that degree reaches system suitability requirement, the ratio of mobile phase is suitably have adjusted, to shorten the time of check analysis.
3rd, assay method:
Mobile phase:Using water as mobile phase A, using acetonitrile as Mobile phase B, the regulation according to the form below carries out gradient elution;Chromatogram Post:C18Post (50mm × 4.6mm, 5 μm);Detection wavelength:203nm;Column temperature:40℃;Flow velocity:1.0ml/min;Sampling volume:20μ l。
4th, prepared by reference substance solution:
(1) reference substance stock solution takes reference substance ginsenoside Rb1, it is accurately weighed, add methanol that every 1ml is made and contain ginsenoside Rb1For 0.15mg solution, produce.
(2) reference substance solution precision measures reference substance stock solution 1ml, puts in 10ml measuring bottles, adds methanol dilution to be shaken to scale It is even, produce.HPLC figures are shown in Fig. 2.
5th, prepared by need testing solution:
This product about 5g is taken, it is accurately weighed, put in conical flask with cover, precision adds methanol 50ml, weighed weight, places At night, put in 80 DEG C of water-baths and be heated to reflux 2 hours, let cool, then weighed weight, the weight of less loss is supplied with methanol, is shaken up, is filtered, Subsequent filtrate is taken, is produced.HPLC figures are shown in Fig. 3.
6th, negative control solution:
According to prescription ratio, the negative preparation without pseudo-ginseng is made by its technique, then press the " system of need testing solution It is standby " prepare negative need testing solution and determine.
HPLC figures are shown in Fig. 4.As a result negative need testing solution with ginsenoside Rb1At the identical retention time of reference substance chromatogram Obvious colour developing spectral peak is had no, therefore thinks noiseless.
7th, linearity and range:
Take ginsenoside Rb1Reference substance 14.52mg, it is accurately weighed, it is placed in 100ml measuring bottles, adds methanol to dissolve and dilute To scale, shake up, as storing solution.Precision measures storing solution 0.25,0.5,1.0,2.0,3.0ml, is respectively placed in 10ml measuring bottles In, with methanol dilution to scale, shake up, obtain the reference substance solution of various concentrations, the accurate 20 μ l that draw press assay bar respectively Part sample introduction determines, and with sample introduction concentration (mg/ml) for abscissa, peak area (A) is ordinate, carries out linear regression, the results are shown in Table 1。
The linearity and range of table 1 tests measurement result
As a result show:Ginsenoside Rb1Have in the range of 3.4013~40.8157 μ g/ml with peak area good linear Relation.
8th, precision:
Reference substance solution under linear term (13.6052 μ g/ml) is taken, by above-mentioned chromatographic condition sample introduction, replication 6 times, note Record ginsenoside Rb1Peak area.
It the results are shown in Table 2.
The precision test measurement result of table 2
As a result show:Ginsenoside Rb1Peak area average deviation is 0.33%, less than 1.0%, illustrates that instrument precision is good It is good, meet the requirement of assay.
9th, replica test:
6 parts of content in freckle cream sample is taken, sample is prepared by need testing solution preparation method, by above-mentioned chromatographic condition sample introduction, every part Enter 2 pins, record ginsenoside Rb1Peak area, calculate ginsenoside Rb1Content.
It the results are shown in Table 3.
The replica test measurement result of table 3
As a result show:Ginsenoside Rb1Average content is 0.1088mg/g, RSD 0.52%, less than 1.0%, shows this The repeatability of method is good.
10th, the rate of recovery:
This product content in freckle cream about 5g is taken, it is accurately weighed, parallel 3 parts, respectively by sample size-reference substance addition substantially (1: 1) ratio adds a certain amount of reference substance solution, is prepared and is surveyed by the preparation method and chromatographic condition of need testing solution It is fixed, content is calculated, the results are shown in Table 4.
The recovery test measurement result of table 4
As a result show:Ginsenoside Rb1Average recovery rate is 98.18%, RSD 1.16%, and it is good to show that this method has The good rate of recovery.
11st, sample size determines:
Three batches of content in freckle cream samples are taken, prepares, produces by the preparation method of need testing solution.By above-mentioned chromatographic condition, every part Sample enters two pins, per the μ l of pin 20, calculates content.
As a result it is as follows:
The sample size measurement result of table 5
12nd, stability:
Content in freckle cream sample is taken, sample is prepared by need testing solution method, sample introduction is distinguished in 0,4,8,12,24h, records ginseng Saponin(e Rb1Peak area.
It the results are shown in Table 6.
The stability test measurement result of table 6
As a result show:Need testing solution had preferable stability in 24 hours.
Test example 3:Skin irritation test:
After the product content in freckle cream of the method preparation gained of this experiment mainly observation embodiment 1 is to the multiple stimulation of guinea pig skin Excitant.
1st, materials and methods:
1.1 animal:Albino guinea-pig, 250~300g of body weight, male and female half and half, provided by Beijing academy of traditional Chinese medicine animal center. Constant temperature (20 ± 1 DEG C), relative humidity are 30~70%, natural lighting, packet raising, feed with common dry greenfeed block, freely drink Water.
1.2 medicine:Content in freckle cream, according to embodiments of the present invention 1 method prepare gained.
1.3 method:By the Ministry of Public Health《New drug preclinical study guideline》Method (4), 24 hours before experiment, cavy the back of the body With 4 × 5cm of hair remover depilation at left and right sides of portion2.Left side is the tested area of normal skin, right side is the tested area of damaged skin.It is every kind of Identical medicine is applied in 6 cavys of observed drug, the tested area of normal skin and the tested area of damaged skin, and (the tested area of damaged skin is in the topical application of drug Preceding to draw " # " in topical application of drug area skin with No. 7 syringe needles, to scratch epidermis, not bleeding is advisable scratch depth).On the left of every cavy just Normal tested skin area and the tested area of right side damaged skin, each each topical application of drug 0.5-1.0g, are uniformly applied on skin of unhairing, daily one It is secondary, successive administration 7 days.Daily O&E local skin whether there is erythema, oedema, by the scale of table 7;Visually can when having When seeing lesion, Ze Xuzuo histopathologic examinations, and press the scale of table 8;Stimulus intensity is finally judged according to table 9.Set simultaneously White (bare substrate) parallel control experiment of one group of blank.
The skin wound repair of table 7 scores
The skin irritation test pathologic diagnosis result standards of grading of table 8
Note:1. total score is by (a+b+c+d+e+f+g)+(i+j+k) or (h)+(i+j+k) selection total score the greater.2. dissociate Refer to collagenous fibres and be separated into fractionlet
The skin irritatin intensity evaluation of table 9
2nd, result:
As shown in table 10, content in freckle cream successive administration 3 days, locally there is slight erythema in 1 male guinea pig, according to skin irritatin Standards of grading are reacted, are integrated as 1 point, continue medication, erythema gradually mitigates, Lock-out after 3 days.All animals during off-test Skin visual inspection is normal, the animal of slight erythema locally occurs because stimulating lighter, Wei Zuo histopathologic examinations.Blank White group has no any other change, identical with the skin of the non-coating of surrounding.
The content in freckle cream of table 10 is to scheming the suitable multiple irritant test of skin
Note:* there is slight stimulation in 1 animal
Test example 4:Content in freckle cream treats 50 clinical observation on the therapeutic effect of chloasma:
To describe therapeutic effect possessed by a kind of compound skin cream for treating chloasma of the present invention in detail, below The effect of content in freckle cream treats chloasma and security are evaluated by clinical observation.
First, research method
(1), test method:Clinical observation is carried out using random opening method.
(2), administrated method, daily after cleaning face, content in freckle cream is applied at night, one month is a course for the treatment of, totally 3 treatments Journey.
(3), testing program:
1st, case selection:
(1), case inclusion criteria:1 is diagnosed as chloasma faciei, age 18-65 year, sex according to typical clinical manifestation It is unlimited.Not used any related drugs in 2 liang of weeks.3 voluntarily receive this clinical test, and by regulation coating and periodic review person.
(2), case exclusion standard:1 high quick constitution or once to a variety of external used medicine allergy sufferers.2 suffer from other maxillofacial diseases Hinder quality or observer.3 suffer from infectious disease or mental illness person.4 gestation and women breast-feeding their children.
(3), case rejects standard:Occur local excitation or allergic reaction during 1 medication.2 can not be completed by agreement for some reason Whole curers.
2nd, parameters for observation on effect and judgement:
(1), parameters for observation on effect:
Facial skin lesion area standards of grading.0=is without skin lesion;1=skin lesion areas<5%;2=skin lesion areas<10%;3=skins Damage area 10-20%;4=skin lesion areas 20-30%;5=skin lesion areas 30-40%;6=skin lesion areas>50%.
Skin lesion and severity scale
Q=quantity, C=colors;0=is harmless, and 1=is slight.2=moderates, 3=severes.
Chloasma faciei order of severity total score=area scoring × (quantity scoring+color score)
(2), the standard of curative effect evaluation:
Base is cured:The skin being grievously injured degree total score reduces at the end of the course for the treatment of>90%
It is effective:The skin being grievously injured degree total score reduces 60-89% at the end of the course for the treatment of
Effectively:The skin being grievously injured degree total score reduces 21-59% at the end of the course for the treatment of
It is invalid:The skin being grievously injured degree total score reduces at the end of the course for the treatment of<20%
Effective percentage=base is cured number of cases+effective number of cases+effectively number of cases/qualified number of cases * 100%
2nd, result
(1), general information:
50 are observed altogether, and case-data is as shown in table 11.
The case-data of table 11
(2), curative effect
1st, pretherapy and post-treatment the skin being grievously injured degree scoring:As a result it is as shown in table 12.
The pretherapy and post-treatment the skin being grievously injured degree scoring (X ± SD) of table 12
2nd, pretherapy and post-treatment the skin being grievously injured degree scoring rate of descent:As a result it is as shown in table 13.
The pretherapy and post-treatment the skin being grievously injured degree scoring rate of descent of table 13
3rd, chloasma therapeutic evaluation is treated:As a result shown in table 14.
Table 14 treats chloasma therapeutic evaluation
It is described above, only presently preferred embodiments of the present invention, not the present invention is made it is any in form and substantial limit System, all those skilled in the art, without departing from the scope of the present invention, when using disclosed above skill Art content, and the equivalent variations for a little variation, modification and evolution made, it is the equivalent embodiment of the present invention;Meanwhile it is all according to The variation, modification and evolution for any equivalent variations made according to the substantial technological of the present invention to above example, still fall within this In the range of the technical scheme of invention.

Claims (4)

  1. A kind of 1. compound skin cream for treating chloasma, it is characterised in that:The compound skin cream is by following The raw material of parts by weight is made:0.25 part of 2.4 parts of pseudo-ginseng, 0.2 part of the flower bud of lily magnolia, 0.14 part of safflower, oil phase, aqueous phase and ginger extrait;
    The oil phase is made from the following raw materials in parts by weight:1.5 parts of dimeticones, 2 parts of Ak6,1 part of Ak25,4 parts of octadecyl alcolol, list, 2 parts of bi-tristearin, 1 part of beeswax, 0.8 part of stearic acid, 8 parts of light liquid petrolatum.
    The aqueous phase is made from the following raw materials in parts by weight:65.83 parts of 12 parts of glycerine, 0.25 part of ethyl hydroxy benzoate and purified water.
  2. 2. a kind of preparation method for being used to treat the compound skin cream of chloasma, comprises the steps:
    (1), the preparation of pseudo-ginseng medicinal extract:2.4 parts of pseudo-ginseng is taken, soaks 2h, then boils and carries 2 times, the 1st time plus 8 times of amounts of water, is decocted 1.5h, the 2nd time plus 6 times of water amount decoct 1h, extract solution filtration, merging filtrate, are concentrated under reduced pressure into about per ml equivalent to 1g medicinal materials, Stirring is lower to add 2 times of amount ethanol, refrigerates 48h, separates supernatant, reclaims ethanol and be concentrated into the leaching that every g medicinal extract contains 2g medicinal materials Cream, pseudo-ginseng medicinal extract is produced, it is standby;
    (2), the preparation of safflower medicinal extract:0.14 part of safflower is taken, soaks 2h, then boils and carries 2 times, the 1st time plus 8 times of amounts of water, is decocted 1.5h is boiled, the 2nd time plus 6 times of amounts of water, 1h is decocted, extract solution filtration, merging filtrate, is concentrated under reduced pressure into about per ml equivalent to 1g medicines Material, lower 2 times of amount ethanol of addition are stirred, 48h is refrigerated, separates supernatant, reclaim ethanol and be concentrated into every g medicinal extract and contain 2g medicinal materials Medicinal extract, safflower medicinal extract is produced, it is standby;
    (3), the preparation of flower bud of lily magnolia medicinal extract:0.2 part of the flower bud of lily magnolia is taken, adds 70% ethanol to soak 1h, is then refluxed for extracting 2 times, the 1st time plus alcohol 8 times of amounts, flow back 1.5h, and the 2nd time plus 6 times of amounts of alcohol, flow back 1h, extract solution filtration, merging filtrate, ethanol is recovered under reduced pressure, and concentrate Contain the medicinal extract of 2g medicinal materials, as flower bud of lily magnolia medicinal extract to every g medicinal extract, it is standby;
    (4), the preparation of oil phase:Raw material, 1.5 parts of dimeticones, 2 parts of Ak6,1 part of Ak25, octadecyl alcolol 4 are weighed by following parts by weight Part, 2 parts of single, double tristerin, 1 part of beeswax, 0.8 part of stearic acid, 8 parts of light liquid petrolatum;By octadecyl alcolol, beeswax, light Matter liquid paraffin, dimeticone, Ak25, Ak6, stearic acid and single, double tristerin, put into oil cauldron, and 80-85 DEG C of water-bath adds Hot melt turns to oil phase, and 80-85 DEG C of insulation is standby;
    (5), the preparation of aqueous phase:Raw material, 12 parts of glycerine, 0.25 part of ethyl hydroxy benzoate, purified water 65.83 are weighed by following parts by weight Part;It is aqueous phase that glycerine, purified water, which are dissolved by heating, when being heated to 60 DEG C, spreads addition ethyl hydroxy benzoate slowly;
    (6), emulsify:The oil phase and heated aqueous of step (4) and (5) preparation gained are simultaneously stirred to 80-85 DEG C, and main cooker is heated to 50-60 DEG C, oil phase is first pumped into main cooker by aqueous phase suction main cooker and after crossing 120 mesh sieves and crosses 120 mesh sieves, opens and stirs 35.0HZ, emulsify frequency 50.0HZ, emulsification times 20 minutes;
    (7), main cooker is heated to the product for adding step (1), step (2) and step (3) after 60 DEG C, emulsifies frequency 50.0HZ, emulsification 20 minutes time;Insulated and stirred frequency 35.0HZ, mixing time 20 minutes;At equal temperature, it is transferred in high pressure homogenizer, The circle of circulation 3 under 10000psi newborn even pressure, takes out, and leads to cooling water temperature, and temperature is down to less than 50 DEG C, and stirring frequency is 30.0HZ;
    (8), temperature is down to 55 DEG C, adds the ginger extrait that parts by weight are 0.25 part;Temperature is down to 37 DEG C of dischargings, produces for controlling Treat the compound skin cream of chloasma.
  3. A kind of 3. compound skin cream for being used to treat chloasma, it is characterised in that:The compound skin cream by Preparation method described in claim 2 prepares gained.
  4. 4. a kind of compound skin cream for being used to treat chloasma described in claim 1 or 3 is preparing treatment chloasma Application in medicine.
CN201711158919.3A 2017-11-20 2017-11-20 A kind of compound skin cream for treating chloasma, preparation method and application Pending CN107823260A (en)

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CN109745361A (en) * 2018-11-08 2019-05-14 戴博 It is a kind of to alleviate senile skin itch and the compound skin cream and its preparation method and application with moisturizing effect

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