CN100404047C - Medicinal composition for treating acne and eczema and its preparing method - Google Patents
Medicinal composition for treating acne and eczema and its preparing method Download PDFInfo
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- CN100404047C CN100404047C CNB2005100870072A CN200510087007A CN100404047C CN 100404047 C CN100404047 C CN 100404047C CN B2005100870072 A CNB2005100870072 A CN B2005100870072A CN 200510087007 A CN200510087007 A CN 200510087007A CN 100404047 C CN100404047 C CN 100404047C
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Abstract
The present invention discloses a kind of compound Chinese medicine preparation for treating acne and eczema and its preparation process. The compound Chinese medicine preparation is prepared with honeysuckle, dandelion, armand, rehmannia root, skullcap root and other several kinds of Chinese medicinal materials. The present invention also provides the quality control method and application in treating acne and eczema of the compound Chinese medicine preparation.
Description
Invention field
The present invention relates to a kind of pharmaceutical composition and preparation method thereof and method of quality control, particularly a kind of pharmaceutical composition for the treatment of acne and eczema and preparation method thereof and method of quality control.
Background technology
Acne vulgaris (AcneVulgaris) is the common a kind of hair follicle of adolescence, sebaceous gland chronic inflammatory disease dermatoses, good sending out in face, multiple infringements such as acne, pimple, pus born of the same parents, tuberosity, cyst and cicatrix are arranged, and, be commonly called as " acne ", " skin sore ", " acne " etc. often with seborrhea.Primary disease was fallen ill in pubarche, be more common in 15～30 years old youth of both sexes, the traditional Chinese medical science claims " Cuo ", " acne ", " rosacea caused by lung-wind ", and the primary disease incidence rate is higher, and the course of disease is touching, often down here, the new continuous secondary of skin ulcer, the delayed several years that has is one of clinical difficult disease, and can leave over the pigmentation speckle and the cicatrix of pitchy, often influence attractive in appearance.
Summary of the invention
The object of the invention is to provide a kind of compound Chinese medicinal preparation for the treatment of acne and eczema and preparation method thereof, and another purpose of the present invention is to provide the method for quality control and the purposes of this Chinese medicinal composition preparation.
The present invention seeks to be achieved through the following technical solutions:
The present invention forms by following 12 flavor raw materials:
Flos Lonicerae 40-60 weight portion Herba Taraxaci 40-60 weight portion
Caulis Clematidis Armandii 180-220 weight portion Radix Rehmanniae 120-160 weight portion
Radix Scutellariae 120-160 weight portion Radix Scrophulariae 80-120 weight portion
Cortex Phellodendri 40-60 weight portion Radix Et Rhizoma Rhei 80-120 weight portion
Fel Sus domestica 10-20 weight portion Margarita layer powder 2-5 weight portion
Cornu Saigae Tataricae powder 0.5-2 weight portion Pulvis Cornus Bubali Concentratus 8-12 weight portion
The best proportioning of above-mentioned 12 flavor crude drug is as follows:
Flos Lonicerae 50 weight portion Herba Taraxacis 50 weight portion Caulis Clematidis Armandiis 200 weight portions
Radix Rehmanniae 150 weight portion Radix Scutellariaes 150 weight portion Radix Scrophulariaes 100 weight portions
Cortex Phellodendri 50 weight portion Radix Et Rhizoma Rhei (wine stir-fry) 100 weight portion Fel Sus domestica 15 weight portions
Margarita layer powder 3 weight portion Cornu Saigae Tataricae powders 1 weight portion Pulvis Cornus Bubali Concentratus 10 weight portions
Can also in the above-mentioned raw materials medicine, add following three flavor crude drug:
Radix Angelicae Sinensis 40-60 weight portion Radix Glehniae 40-60 weight portion Radix Paeoniae Rubra 40-60 weight portion
The best proportioning of the three flavor crude drug that also can add is:
Radix Angelicae Sinensis 50 weight portion Radix Glehniaes 50 weight portion Radix Paeoniae Rubra 50 weight portions
Above-mentioned composition can be made tablet, soft capsule, capsule, slow releasing agent, granule, drop pill, oral liquid or lyophilized injectable powder.
The concrete preparation technology of the present invention's 12 flavor crude drug is as follows:
The Radix Scutellariae of extracting honeysuckle, Herba Taraxaci, Caulis Clematidis Armandii, Radix Rehmanniae, 2/3 weight portion, Radix Scrophulariae, Cortex Phellodendri, Radix Et Rhizoma Rhei add up pharmaceutical composition weight 8-12 decocting doubly and boil 2-4 time, filter merging filtrate, add Fel Sus domestica and stir evenly, be condensed into thick paste, drying, be ground into fine powder A, standby; The Radix Scutellariae powder of residue 1/3 weight portion is broken into fine powder B, with fine powder A, fine powder B, Margarita layer powder, Cornu Saigae Tataricae powder, Pulvis Cornus Bubali Concentratus mixing; Add conventional adjuvant granulation or encapsulated.
The concrete preparation technology of the present invention's ten five tastes crude drug is as follows:
The Radix Scutellariae of extracting honeysuckle, Herba Taraxaci, Caulis Clematidis Armandii, Radix Angelicae Sinensis, Radix Rehmanniae, 2/3 weight portion, Radix Scrophulariae, Cortex Phellodendri, Radix Et Rhizoma Rhei add up pharmaceutical composition weight 8-12 decocting doubly and boil 2-4 time, filter merging filtrate, add Fel Sus domestica and stir evenly, be condensed into thick paste, drying, be ground into fine powder A, standby; The Radix Scutellariae powder of Radix Glehniae, Radix Paeoniae Rubra and residue 1/3 weight portion is broken into fine powder B, with fine powder A, fine powder B, Margarita layer powder, Cornu Saigae Tataricae powder, Pulvis Cornus Bubali Concentratus mixing. add conventional adjuvant granulation or encapsulated.
Method of quality control of the present invention comprises following discrimination method and/or content assaying method
Discrimination method comprises one or more in the following discriminating:
A, get agent of this medicament composition capsule or granule, put microscopically and observe: fiber is faint yellow, fusiformis, and wall thickness, the hole ditch is thin; Calcium oxalate cluster crystal diameter 7～38 μ m; Secretory canal includes the yellowish-brown thing, and is how broken, is lumps; Irregular fragment is colourless, and is translucent, visible sometimes fine and closely woven wavy grain;
B, get the agent of this medicament composition capsule or granule day taking dose 5/9, add methanol 20-40ml supersound process 10-20 minute, filter, the filtrate evaporate to dryness, residue adds water 15-25ml makes dissolving, and regulating pH value with hydrochloric acid is 1～2, adds ethyl acetate extraction 1-3 time, each 20-40ml, merge the cruel liquid of acetic acid second, water 10-20ml washing, evaporate to dryness, residue adds dehydrated alcohol 1ml makes dissolving, as need testing solution; Other gets the baicalin reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw each 5 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with 5-8: 2-4: ethyl acetate-butanone of 1: 1-formic acid-water is developing solvent, pre-equilibration 20-40 minute, launch, take out, dry, spray is with in 1-3% ferric chloride alcoholic solution, the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
C, get Radix Et Rhizoma Rhei control medicinal material 0.1g, add methanol 15-25ml dipping 0.5-1.5 hour, filter, get filtrate 3-7ml, evaporate to dryness, residue add water 8-12ml makes dissolving, add hydrochloric acid 1ml again, put in the water-bath and heated 20-40 minute, immediately cooling, add diethyl ether and extract 1-3 time, each 15-25ml merges ether solution, evaporate to dryness, residue adds dehydrated alcohol 1ml makes dissolving, in contrast medical material solution; Other gets the emodin reference substance, adds dehydrated alcohol and makes the solution that every 1ml contains 0.5mg, in contrast product solution; Test according to thin layer chromatography, draw need testing solution and each 5 μ l of above-mentioned two kinds of solution of differentiating under the B item, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with 5-7: 2: 0.1 normal hexane one ethyl acetate one formic acid is developing solvent, launch, take out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show identical orange-yellow fluorescence principal spot: with the corresponding position of reference substance chromatograph on, show identical orange-yellow fluorescence speckle, put in the ammonia smoked after, inspect under the daylight, speckle becomes redness;
D, get agent of this medicament composition capsule or granule the day taking dose 5/9, add methanol 20-40ml, supersound process 10-20 minute, filter, the filtrate evaporate to dryness. residue adds water 15-25ml makes dissolving, extracts the extracting solution evaporate to dryness with water saturated n-butyl alcohol 20-40ml, residue adds methanol 1ml makes dissolving, add neutral alumina 1g, in water-bath, mix thoroughly, drying, be added on 100～200 purpose neutral alumina posts, with ethanol 40-60ml eluting, collect eluent, evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution; Other gets Cortex Phellodendri control medicinal material 0.1g, shines medical material solution in pairs with legal system; Get the berberine hydrochloride reference substance again, add methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution; According to thin layer chromatography test, draw each 1 μ l of above-mentioned three kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with 6-8: n-butyl alcohol-glacial acetic acid of 1: 2-water is developing solvent, launches, and takes out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show identical yellow fluorescence speckle;
E, get the peoniflorin reference substance, add methanol and make the solution that every 1ml contains 2mg, in contrast product solution; Test according to thin layer chromatography, prepare test sample and reference substance with reference to the C item, draw each 4 μ l of need testing solution and reference substance solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with 38-43: 5: 9-12: chloroform-ethyl acetate of 0.2-methanol-formic acid is developing solvent, launches, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to speckle colour developing; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical bluish violet speckle.
Content assaying method in the method for quality control is as follows
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; With 40-45: 55-60: 0.2 methanol-water-phosphoric acid is a mobile phase: the detection wavelength is 280nm, and number of theoretical plate calculates by the baicalin peak and is not less than 2000;
The preparation of reference substance solution: it is an amount of that precision takes by weighing the baicalin reference substance, adds methanol and make the solution that every 1ml contains 60 μ g, promptly;
The preparation of need testing solution: get the content of agent of this medicament composition capsule or granule, porphyrize is got 0.2-0.4g, and accurate the title decides, put in the tool plug conical flask, the accurate 60-80% ethanol 45-55ml that adds claims to decide weight, supersound process 20-40 minute, put coldly, claim to decide weight again, supply the weight that subtracts mistake with 60-80% ethanol, shake up, filter, the accurate filtrate 5ml that draws to the 10ml measuring bottle, adds 60-80% ethanol to scale, shake up, filter, promptly;
Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly;
The per diem taking dose meter of agent of this medicament composition capsule or granule contains Radix Scutellariae with baicalin C
21H
18O
11Must not be less than 54mg.
Preparation of the present invention comprises dosage forms such as capsule or granule, and every day, dose was equivalent to primary dose 8.646-14.148g.
It is monarch drug that this pharmaceutical composition is reused Radix Scutellariae, Radix Et Rhizoma Rhei, Caulis Clematidis Armandii; Be aided with Flos Lonicerae, Herba Taraxaci, Radix Scrophulariae, Cortex Phellodendri, Fel Sus domestica heat-clearing and toxic substances removing, Radix Rehmanniae, Margarita layer powder, Cornu Saigae Tataricae powder, Pulvis Cornus Bubali Concentratus clearing away heat and cooling blood are ministerial drug; Can also help in the compositions with Radix Angelicae Sinensis, Radix Paeoniae Rubra blood circulation and channel invigorating, Radix Glehniae is protected stomach-Yin, the moon in case group's bitter cold medicine injures one's stomach.All medicines share, and it is damp and hot to be Qinghua altogether, the agent that heat-clearing and toxic substances removing, removing heat from blood are promoted blood circulation, for eczema " damp-heat syndrome ", acne " damp-heat syndrome ", dermatitis " damp-heat syndrome " use all suitable.Dialectical main points are all gastrointestinal excess-heat (seeing diseases such as constipation dark coloured urine), heat in blood (the skin lesion place is red, swollen, bitterly, red tongue, rapid pulse etc. is seen disease) persons that possess, and all belong to the indication category.All medicines share, treatment acne good effect, and few side effects is worth clinical expansion to use.
In method of quality control, measure the selection of wavelength: get baicalin reference substance solution (60 μ l/ml), in the interscan of 230～430nm wave-length coverage, the result 279 (± 1nm) there is absorption maximum at the wavelength place.
The selection of mobile phase: through suitable proportioning, the ratio of mobile phase is with methanol-water-phosphoric acid (42: 58: 0.2), and baicalin peak and adjacent peak separating degree are better.
Blank assay: get the scarce Radix Scutellariae negative sample 0.3g in prescription ratio and method for making preparation, handle and measure by the preparation and the assay method of need testing solution, the HPLC collection of illustrative plates does not see that blank assay has interference as a result.
The precision test: the accurate baicalin reference substance solution 10 μ l that draw, press content assaying method and repeat sample introduction 5 times, measure the absworption peak area.The meansigma methods of peak area is 1413245, and RSD% shows that all less than 0.74% 5 sample introduction phase similarities do not have obvious variation mutually, and the precision of instrument is good.
Replica test: get same test sample, porphyrize, precision takes by weighing 5 parts, presses content assaying method and measures.The content meansigma methods is 6.60, and RSD% is 1.33, illustrates that the repeatability of this method is good.
Stability test: accurate same reference substance solution (60.8 μ g/ml) and the need testing solution drawn, after start was waited to stablize in 1 hour,, inject high performance liquid chromatograph respectively at 0,2,4,6 and 12 hour, press content assaying method and measure peak area.Reference substance peak area meansigma methods 1374948, test sample peak area meansigma methods 1728364, reference substance RSD% is 0.55, test sample RSD% is 1.32, illustrates that reference substance and need testing solution were stable in 12 hours.
Application of sample recovery test: get test sample (lot number: 20031201, contain baicalin 20.73mg/g) porphyrize, get 5 parts of each 0.3g, the accurate title, decide, accurate baicalin reference substance solution (6.04mg/ml) 1ml that adds, water-bath volatilizes, measure by the above-mentioned content assaying method of drafting, average recovery rate is 98.28, and average RSD% is 0.61.
Sample size is measured: measure three batch samples by method under the assay item, calculate wherein content of baicalin with external standard method, average content (mg/ grain) is 6.26, but moisture content in the consideration sample and content uniformity are made the error of content of baicalin, in conjunction with above-mentioned result of the test, every (heavy 0.3g) contains Radix Scutellariae with baicalin (C
21H
18O
11) meter, must not be less than 4.5mg.
Following experimental example is used to further specify but is not limited to the present invention.
Experimental example 1: the preparation experiment of standard curve
Baicalin reference substance (715-200111 is for assay usefulness, Nat'l Pharmaceutical ﹠ Biological Products Control Institute).Methanol: chromatographically pure; Water; Ultra-pure water; Other reagent: be analytical pure.The stainless steel column of Hypersil ODS (4.6 * 200mm, 5 μ m); Mobile phase: methanol-water-phosphoric acid (42: 58: 0.2) flow velocity: 1.0ml/min; Detect wavelength: 280nm; Column temperature; Room temperature.
The preparation of reference substance solution: (715-200111 (using) Nat'l Pharmaceutical ﹠ Biological Products Control Institute) reference substance heavy (g): 0.0152 for assay
Adding methanol is diluted to: 10ml
(1) the accurate 1ml → 10ml (152.0mg/ml) that draws
(2) the accurate 0.8ml → 10ml (121.6mg/ml) that draws
(3) the accurate 0.6ml → 10ml (91.2mg/ml) that draws
(4) the accurate 1ml → 25ml (60.8mg/ml) that draws
(5) the accurate 1ml → 10ml (30.4mg/ml) that draws
Measure: draw 10 μ l respectively, press content assaying method and measure peak area.The results are shown in following table.
Table
| C(μl/ml) | 30.4 | 60.8 | 91.2 | 121.6 | 152.0 |
| Peak area | 858824 | 1539838 | 2305267 | 3096220 | 3871557 |
As abscissa, the peak area A that records carries out linear regression as ordinate with reference substance concentration W, linear equation: Y=2E+06 *+59787r=0.9996
The range of linearity: 30.4～152.0 μ g
Experimental example 2: the preparation test of need testing solution
Extracting method () under " Radix Scutellariae " assay item is: get about 0.3g, the accurate title, decide, add 70% ethanol 40ml, reflux 3 hours is put cold, filter, filtrate is put in the 100ml measuring bottle, and with a small amount of 70% ethanol gradation washing container and residue, washing liquid is filtered in the same measuring bottle, add 70% ethanol to scale, shake up.
According to above-mentioned preparation method, get this product 0.3g respectively, the accurate title, decide, and tests as follows: 20 weights of sample (g): 5.8281; Average particle heavy (g): 0.2914; Reference substance concentration: 59.0mg/ml; Make need testing solution A.Test sample heavy (g): 0.3049
Extracting method (two): the accurate 70% ethanol 50ml that adds claims to decide weight, reflux 1 hour, put coldly, claim again to decide weight, supply the weight that subtracts mistake with 70% ethanol, shake up, filter, the accurate filtrate 5ml that draws is to the 10ml measuring bottle, add 70% ethanol to scale, shake up, filter, make need testing solution B. test sample heavy (g): 0.3062
Press extracting method () preparation, ultrasonic 20 minutes, 30 minutes, 60 minutes respectively, make need testing solution C, D, E.Wherein, heavy (g): the C 0.3104 of test sample, D 0.3055, and E 0.2991
4, measure: draw each 10 μ l of above-mentioned solution respectively, press content assaying method and measure content of baicalin
| Need testing solution | A | B | C | D | E |
| Content (mg/ grain) | 7.18 | 7.20 | 7.06 | 7.19 | 7.16 |
Above method, result of the test content is basic identical, all the baicalin in the sample can be extracted fully, and in conjunction with application of sample recovery test result, the supersound extraction that selection operation is comparatively simple and direct is as the preparation method of need testing solution.
Experimental example 3: Radix Scutellariae thin layer chromatography discrimination method
Instrument and reagent: KQ-100 type ultrasonic cleaner; Baicalin reference substance (calibrating of 715-200111 Chinese biological goods provides); (chemical pure, Qingdao Marine Chemical Co., Ltd. makes tlc silica gel G, lot number: 031215): ethyl acetate etc.: be analytical pure.
The preparation of need testing solution: get this product content 2g, add methanol 30ml supersound process 15 minutes, filter, the filtrate evaporate to dryness, residue adds water 20ml makes dissolving, and regulating pH value with hydrochloric acid is 1-2, adds ethyl acetate extraction 2 times, each 30ml, merge ethyl acetate liquid, water 15ml washing, evaporate to dryness, residue adds dehydrated alcohol 1ml makes dissolving, as need testing solution.
The preparation of reference substance solution: get the baicalin reference substance, add methanol and make the solution that every 1ml contains 1mg, in contrast product solution.
The preparation of negative control solution: make the negative sample that lacks Radix Scutellariae in prescription ratio and method for making, get 2g, press the preparation method of test sample, make the negative control solution that lacks Radix Scutellariae.
Thin layer chromatography: according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000) test, draw each 5 μ l of above-mentioned three kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with ethyl acetate-butanone-formic acid-water (6: 3: 1: 1) be developing solvent, pre-equilibration 30 minutes, room temperature is launched, exhibition is apart from 8cm, take out, dry, spray is with 2% ferric chloride alcoholic solution.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.The negative control chromatograph is noiseless on the relevant position.
Experimental example 4: the thin layer chromatography discrimination method of Radix Et Rhizoma Rhei
Instrument and reagent: KQ-100 type ultrasonic cleaner; Radix Et Rhizoma Rhei control medicinal material (calibrating of 902-8901 Chinese biological goods provides); Emodin reference substance (calibrating of 110756-200110 Chinese biological goods provides): (chemical pure, Qingdao Marine Chemical Co., Ltd. makes tlc silica gel G, lot number: 031215): methanol etc.: be analytical pure.
The preparation of need testing solution: differentiate the item preparation method of need testing solution down with Radix Scutellariae.
The preparation of control medicinal material solution: get Radix Et Rhizoma Rhei control medicinal material 0.1g, add methanol 20ml dipping 1 hour, filter, get filtrate 5ml, evaporate to dryness, residue add water 10ml makes dissolving, add hydrochloric acid 1ml again, put in the water-bath and heated 30 minutes, immediately cooling, with ethyl acetate extraction 2 times, each 20ml merges ethyl acetate liquid, evaporate to dryness, residue adds dehydrated alcohol 1ml makes dissolving, in contrast medical material solution.
The preparation of reference substance solution: get the emodin reference substance, add dehydrated alcohol and make the solution that every 1ml contains 0.5mg, in contrast product solution.
The preparation of negative control solution: make the negative sample that lacks Radix Et Rhizoma Rhei in prescription ratio and method for making, get 2g, press the preparation method of test sample, make the negative control solution that lacks Radix Et Rhizoma Rhei.
Thin layer chromatography, test according to thin layer chromatography, draw each 5 μ l of above-mentioned four kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with normal hexane one ethyl acetate, one formic acid (6: 2: 0.1), room temperature is launched, exhibition is apart from 8cm, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the control medicinal material chromatograph near on 3 speckle relevant positions in forward position, show identical orange-yellow fluorescence principal spot; With the corresponding position of reference substance chromatograph on, show identical orange-yellow fluorescence speckle, put in the ammonia smoked after, inspect under the daylight, speckle becomes redness.The negative control chromatograph is noiseless on the relevant position.
The developing solvent that pharmacopeia is recorded is petroleum ether (30～60 ℃)-Ethyl formate-formic acid (15: 5: 1), through comparing, with normal hexane one ethyl acetate, one formic acid (6: 2: 0.1) is that developing solvent is more stable than the former character, and the chromatograph repeatability is better, and relative temperature is controlled at below 50% to well during expansion.
Experimental example 5: the thin layer chromatography discrimination test of Cortex Phellodendri
Instrument and reagent: KQ-100 type ultrasonic cleaner: Cortex Phellodendri control medicinal material (calibrating of 0937-9703 Chinese biological goods provides); Berberine hydrochloride reference substance (calibrating of 0713-9906 Chinese biological goods provides); (Shanghai the May 4th chemical reagent company limited, lot number: 020402) (chemical pure, Qingdao Marine Chemical Co., Ltd. makes tlc silica gel G chromatography, lot number: 031215): methanol etc.: be analytical pure with neutral alumina.
The preparation of need testing solution: get this product content 2g, add methanol 30ml supersound process 15 minutes, filter the filtrate evaporate to dryness, residue adds water 20ml makes dissolving, extracts the extracting solution evaporate to dryness with water saturated n-butyl alcohol 30ml, residue adds methanol 1ml makes dissolving, adds neutral alumina 1g, mixes thoroughly in water-bath, drying is added in neutral alumina post (100～200 orders, 3g, internal diameter 1cm) on,, collects eluent with ethanol 50ml eluting, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.
The preparation of control medicinal material solution: get Cortex Phellodendri control medicinal material 0.1g,, make control medicinal material solution with the preparation method of need testing solution.
The preparation of reference substance solution: get the berberine hydrochloride reference substance, add methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution.
The preparation of negative control solution: make the negative sample that lacks Cortex Phellodendri in prescription ratio and method for making, get 2g, press the preparation method of test sample, make the negative control solution that lacks Cortex Phellodendri.
Thin layer chromatography: according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000) test, draw each 1 μ l of above-mentioned four kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with n-butyl alcohol-glacial acetic acid-water (7: 1: 2) is developing solvent, room temperature is launched, and exhibition is taken out apart from 8cm, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show identical yellow fluorescence speckle; The negative control chromatograph on the reference substance relevant position, micro-weak fluorescent orange speckle, but noiseless to the observation of collection of illustrative plates.
In the official method, after sample thief adds methanol eddy, directly as need testing solution.Through test, the collection of illustrative plates after the expansion disturbs big, so increase the little column purification of aluminium oxide, launches back collection of illustrative plates clear spot, disturbs little.Experimental example 6: the thin layer chromatography discrimination test of Radix Paeoniae Rubra
Instrument and reagent: KQ-100 type ultrasonic cleaner: peoniflorin reference substance (calibrating of 0736-98111 Chinese biological goods provides): chromatography neutral alumina (Shanghai the May 4th chemical reagent company limited, lot number: 020402); Tlc silica gel G (chemical pure, Qingdao Marine Chemical Co., Ltd. makes, lot number: 031215); Methanol etc.: be analytical pure.
The preparation of need testing solution: differentiate the item preparation method of need testing solution down with Cortex Phellodendri.
The preparation of reference substance solution: get the peoniflorin reference substance, add methanol and make the solution that every 1ml contains 2mg, in contrast product solution.
The preparation of negative control solution: make the negative sample that lacks Radix Paeoniae Rubra in prescription ratio and method for making, get 2g, press the preparation method of test sample, make the negative control solution that lacks Radix Paeoniae Rubra.
Thin layer chromatography: according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000) test, draw each 4 μ l of above-mentioned three kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, (40: 5: 10: 0.2) be developing solvent, room temperature was launched, and exhibition is apart from 8cm with chloroform-ethyl acetate-methanol-formic acid, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to speckle colour developing.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical bluish violet speckle.The negative control chromatograph is noiseless on the relevant position.
Experimental example 7: this medicament composition capsule agent treatment acne 30 routine observation of curative effect
All patients are the out-patient, all meet " modern skin cypridology diagnosis and treatment handbook diagnostic criteria.Wherein male 12 examples, women 18 examples; Minimum 12 years old of age, maximum 32 years old, average 20.8 years old, the longest 11 years the course of disease the shortest January, average 3.8 years.Not concurrent other dermatosiss of all patient's faces were not used any oral medicine and medicine for external use that influences the acne course of disease in 1 month, do not have serious liver, renal dysfunction person.
With the agent of this medicament composition capsule, each 2, every day 3 times; 2 weeks were a course of treatment, treated 2 courses of treatment altogether, and carried out the course of treatment and observe, record skin lesion situation of change.Respectively check liver function, blood, urine, just conventional 1 time before the treatment and after finishing the course of treatment, judge curative effect 2 courses of treatment.
, greasiness group food sweet, peppery: the cosmetics of stopping using at the period in a medicine diet; Do not eat the food that causes acne: do not contact the factor that excites acne; Maintenance is emotionally stable, optimism.Advise the patient not with hands extruding affected part erythra, diet is suitable light.
With reference to 339 pages of modern combination of Chinese and Western medicine magazine 2002 the 11st the 4th phases of volume about the acne curative effect determinate standard.Total effective rate adds the produce effects meter for recovery from illness.11 examples of fully recovering account for 36.7%, and produce effects 17 examples account for 56.7%; Effective 1 example accounts for 3.3%; Invalid 1 example accounts for 3.3%: total effective rate is 93.4%.Just routine is all no abnormal through looking into liver function and hematuria; Untoward reaction does not appear in the therapeutic process and after the treatment.
Specific embodiment is as follows:
Embodiment 1:The preparation of granule
Flos Lonicerae 45g Herba Taraxaci 55g Caulis Clematidis Armandii 185g Radix Rehmanniae 155g Radix Scutellariae 125g
Radix Scrophulariae 115g Cortex Phellodendri 45g Radix Et Rhizoma Rhei 115g Fel Sus domestica 12g
Margarita layer powder 4g Cornu Saigae Tataricae powder 1g Pulvis Cornus Bubali Concentratus 11g
The decocting that the Radix Scutellariae of extracting honeysuckle, Herba Taraxaci, Caulis Clematidis Armandii, Radix Rehmanniae, 84g, Radix Scrophulariae, Cortex Phellodendri, Radix Et Rhizoma Rhei add 8000g boils 2-4 time, filters, and merging filtrate adds Fel Sus domestica and stirs evenly, and is condensed into thick paste, and drying is ground into fine powder A, and is standby; The Radix Scutellariae powder of residue 1/3 weight portion is broken into fine powder B, with fine powder A, fine powder B, Margarita layer powder, Cornu Saigae Tataricae powder, Pulvis Cornus Bubali Concentratus mixing; Add conventional adjuvant and make granule.
Embodiment 2:Capsular preparation
Flos Lonicerae 55g Herba Taraxaci 45g Caulis Clematidis Armandii 215g Radix Rehmanniae 125g Radix Scutellariae 155g
Radix Scrophulariae 85g Cortex Phellodendri 55g Radix Et Rhizoma Rhei 85g Fel Sus domestica 18g Margarita layer powder 3g
Cornu Saigae Tataricae powder 1.5g Pulvis Cornus Bubali Concentratus 9g Radix Angelicae Sinensis 55g
Radix Glehniae 45g Radix Paeoniae Rubra 55g
Extracting honeysuckle, Herba Taraxaci, Caulis Clematidis Armandii, Radix Angelicae Sinensis, Radix Rehmanniae, 104g Radix Scutellariae, Radix Scrophulariae, Cortex Phellodendri, Radix Et Rhizoma Rhei add up pharmaceutical composition weight 8-12 decocting doubly and boil 2-4 time, filter merging filtrate, add Fel Sus domestica and stir evenly, be condensed into thick paste, drying, be ground into fine powder A, standby; Radix Glehniae, Radix Paeoniae Rubra and residue 51g Radix Scutellariae powder are broken into fine powder B, and with fine powder A, fine powder B, Margarita layer powder, Cornu Saigae Tataricae powder, Pulvis Cornus Bubali Concentratus mixing, it is encapsulated to add conventional adjuvant.The acne and eczema patient is oral, one time 4,3 times on the one.
Embodiment 3:The preparation of tablet
Extracting honeysuckle 45g, Herba Taraxaci 55g, Caulis Clematidis Armandii 185g, Radix Rehmanniae 155g, Radix Scutellariae 125g, Radix Scrophulariae 115g, Cortex Phellodendri 45g, Radix Et Rhizoma Rhei 115g, Fel Sus domestica 12g, Margarita layer powder 4g, Cornu Saigae Tataricae powder 1g, Pulvis Cornus Bubali Concentratus 11g, Radix Angelicae Sinensis 45g, northern husky 55g, Radix Paeoniae Rubra 45g, add conventional adjuvant and make tablet, every heavy 0.3g, acne and eczema the patient take.Each 4, every day 3 times.
Embodiment 4:The preparation of oral administration solution
Extracting honeysuckle 55g, Herba Taraxaci 45g, Caulis Clematidis Armandii 215g, Radix Rehmanniae 125g, Radix Scutellariae 155g, Radix Scrophulariae 85g, Cortex Phellodendri 55g, Radix Et Rhizoma Rhei 85g, Fel Sus domestica 18g, Margarita layer powder 3g, Cornu Saigae Tataricae powder 1.5g, Pulvis Cornus Bubali Concentratus 9g, add conventional adjuvant and make oral administration solution, 10 milliliters every bottle, acne and eczema the patient take, each one bottle, every day 3 times.
Embodiment 5:The preparation of slow releasing tablet
Flos Lonicerae 50g, Herba Taraxaci 50g, Caulis Clematidis Armandii 200g, Radix Rehmanniae 150g, Radix Scutellariae 150g, Radix Scrophulariae 100g, Cortex Phellodendri 50g, Radix Et Rhizoma Rhei (wine stir-fry) 100g, Fel Sus domestica 15g, Margarita layer powder 3g, Cornu Saigae Tataricae powder 1g, Pulvis Cornus Bubali Concentratus 10g, add conventional adjuvant and make slow releasing tablet, every 1g, acne and eczema the patient take, each 1, every day 1 time.
Embodiment 6:The preparation of drop pill
Flos Lonicerae 50g, Herba Taraxaci 50g, Caulis Clematidis Armandii 200g, Radix Rehmanniae 150g, Radix Scutellariae 150g, Radix Scrophulariae 100g, Cortex Phellodendri 50g, Radix Et Rhizoma Rhei (wine stir-fry) 100g, Fel Sus domestica 15g, Margarita layer powder 3g, Cornu Saigae Tataricae powder 1g, Pulvis Cornus Bubali Concentratus 10g, Radix Angelicae Sinensis 50g, Radix Glehniae 50g, Radix Paeoniae Rubra 50g add conventional adjuvant and make drop pill.
Embodiment 7:Discrimination method in the quality control
(1) get embodiment 1 content, put microscopically and observe: fiber is faint yellow, fusiformis, and wall thickness, the hole ditch is thin.Calcium oxalate cluster crystal diameter 7～38 μ m.Secretory canal includes the yellowish-brown thing, and is how broken, is lumps.Irregular fragment is colourless, and is translucent, visible sometimes fine and closely woven wavy grain.
(2) get embodiment 1 content 2g, add methanol 30ml supersound process 15 minutes, filter, the filtrate evaporate to dryness, residue adds water 20ml makes dissolving, and regulating pH value with hydrochloric acid is 1～2, adds ethyl acetate extraction 2 times, each 30ml, merge the cruel liquid of acetic acid second, water 15ml washing, evaporate to dryness, residue adds dehydrated alcohol 1ml makes dissolving, as need testing solution.Other gets the baicalin reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B), draw each 5 μ l of above-mentioned two kinds of solution, put respectively in-be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with ethyl acetate-butanone-formic acid-water (6: 3: 1: 1) be developing solvent, pre-equilibration 30 minutes, launch, take out, dry, spray is with in 2% ferric chloride alcoholic solution, the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
(3) get Radix Et Rhizoma Rhei control medicinal material 0.1g, add methanol 20ml dipping 1 hour, filter, get filtrate 5ml, evaporate to dryness, residue add water 10ml makes dissolving, add hydrochloric acid 1ml again, put in the water-bath and heated 30 minutes, immediately cooling, add diethyl ether and extract 2 times, each 20ml merges ether solution, evaporate to dryness, residue adds dehydrated alcohol 1ml makes dissolving, in contrast medical material solution.Other gets the emodin reference substance, adds dehydrated alcohol and makes the solution that every 1ml contains 0.5mg, in contrast product solution.According to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B) test, draw; Need testing solution under the item of (discriminating) (2) and each 5 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with normal hexane one ethyl acetate, one formic acid (6: 2: 0.1) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show identical orange-yellow fluorescence principal spot: with the corresponding position of reference substance chromatograph on, show identical orange-yellow fluorescence speckle, put in the ammonia smoked after, inspect under the daylight, speckle becomes redness.
(4) get embodiment 1 content 2g, add methanol 30ml, supersound process 15 minutes filters, the filtrate evaporate to dryness. residue adds water 20ml makes dissolving, extracts the extracting solution evaporate to dryness with water saturated n-butyl alcohol 30ml, residue adds methanol 1ml makes dissolving, adds neutral alumina 1g, mixes thoroughly in water-bath, drying is added in neutral alumina post (100～200 orders, 3g, internal diameter 1cm) on,, collects eluent with ethanol 50ml eluting, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets Cortex Phellodendri control medicinal material 0.1g, shines medical material solution in pairs with legal system.Get the berberine hydrochloride reference substance again, add methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000), draw each 1 μ l of above-mentioned three kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with n-butyl alcohol-glacial acetic acid-water (7: 1: 2) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show identical yellow fluorescence speckle.
(5) get the peoniflorin reference substance, add methanol and make the solution that every 1ml contains 2mg, in contrast product solution.According to thin layer chromatography (in be stranded an appendix VI of pharmacopeia version in 2000 B) test, get the capsule of embodiment 2, with reference to [discriminating] (2) preparation test sample, [discriminating] (3) preparation reference substance, draw each 4 μ l of need testing solution and reference substance solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with chloroform-ethyl acetate-methanol-formic acid (40: 5: 10: 0.2) be developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to speckle colour developing.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical bluish violet speckle.
Embodiment 8:Content assaying method in the quality control
The drug combination preparation of getting embodiment 2 carries out assay.
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; With methanol-water-phosphoric acid (42: 58: 0.2) is mobile phase: the detection wavelength is 280nm, and number of theoretical plate calculates by the baicalin peak and is not less than 2000.
The preparation of reference substance solution: it is an amount of that precision takes by weighing the baicalin reference substance, adds methanol and make the solution that every 1ml contains 60 μ g, promptly.
The preparation of need testing solution: get content under the content uniformity item, porphyrize is got 0.3g, and accurate the title decides, put in the tool plug conical flask, the accurate 70% ethanol 50ml that adds claims to decide weight, supersound process 30 minutes is put coldly, claims to decide weight again, supply the weight that subtracts mistake with 70% ethanol, shake up, filter, the accurate filtrate 5ml that draws to the 10ml measuring bottle, adds 70% ethanol to scale, shake up, filter, promptly.
Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly.
Every of this product contains Radix Scutellariae with baicalin (C
21H
18O
11) meter, must not be less than 4.5mg.
Embodiment 9:Method of quality control
(1) get embodiment 2 contents, put microscopically and observe: fiber is faint yellow, fusiformis, and wall thickness, the hole ditch is thin.Calcium oxalate cluster crystal diameter 7～38 μ m.Secretory canal includes the yellowish-brown thing, and is how broken, is lumps.Irregular fragment is colourless, and is translucent, visible sometimes fine and closely woven wavy grain.
(2) get embodiment 2 content 2g, add methanol 30ml supersound process 15 minutes, filter, the filtrate evaporate to dryness, residue adds water 20ml makes dissolving, and regulating pH value with hydrochloric acid is 1～2, adds ethyl acetate extraction 2 times, each 30ml, merge the cruel liquid of acetic acid second, water 15ml washing, evaporate to dryness, residue adds dehydrated alcohol 1ml makes dissolving, as need testing solution.Other gets the baicalin reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B), draw each 5 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with ethyl acetate-butanone-formic acid-water (6: 3: 1: 1) be developing solvent, pre-equilibration 30 minutes, launch, take out, dry, spray is with in 2% ferric chloride alcoholic solution, the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
(3) get Radix Et Rhizoma Rhei control medicinal material 0.1g, add methanol 20ml dipping 1 hour, filter, get filtrate 5ml, evaporate to dryness, residue add water 10ml makes dissolving, add hydrochloric acid 1ml again, put in the water-bath and heated 30 minutes, immediately cooling, add diethyl ether and extract 2 times, each 20ml merges ether solution, evaporate to dryness, residue adds dehydrated alcohol 1ml makes dissolving, in contrast medical material solution.Other gets the emodin reference substance, adds dehydrated alcohol and makes the solution that every 1ml contains 0.5mg, in contrast product solution.According to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B) test, draw; Need testing solution under the item of (discriminating) (2) and each 5 μ of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with normal hexane one ethyl acetate, one formic acid (6: 2: 0.1) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show identical orange-yellow fluorescence principal spot: with the corresponding position of reference substance chromatograph on, show identical orange-yellow fluorescence speckle, put in the ammonia smoked after, inspect under the daylight, speckle becomes redness.
(4) get embodiment 2 content 2g, add methanol 30ml, supersound process 15 minutes filters, the filtrate evaporate to dryness. residue adds water 20ml makes dissolving, extracts the extracting solution evaporate to dryness with water saturated n-butyl alcohol 30ml, residue adds methanol 1ml makes dissolving, adds neutral alumina 1g, mixes thoroughly in water-bath, drying is added in neutral alumina post (100～200 orders, 3g, internal diameter 1cm) on,, collects eluent with ethanol 50ml eluting, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets Cortex Phellodendri control medicinal material 0.1g, shines medical material solution in pairs with legal system.Get the berberine hydrochloride reference substance again, add methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000), draw each 1 μ l of above-mentioned three kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with n-butyl alcohol-glacial acetic acid-water (7: 1: 2) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show identical yellow fluorescence speckle.
(5) get the peoniflorin reference substance, add methanol and make the solution that every 1ml contains 2mg, in contrast product solution.According to thin layer chromatography (in be stranded an appendix VI of pharmacopeia version in 2000 B) test, draw need testing solution and each 4 μ l of reference substance solution under the item of [discriminating] (3), put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with chloroform-ethyl acetate-methanol-formic acid (40: 5: 10: 0.2) be developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical bluish violet speckle.
The drug combination preparation of getting embodiment 1 carries out assay.
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; With methanol-water-phosphoric acid (42: 58: 0.2) is mobile phase: the detection wavelength is 280nm, and number of theoretical plate calculates by the baicalin peak and is not less than 2000.
The preparation of reference substance solution: it is an amount of that precision takes by weighing the baicalin reference substance, adds methanol and make the solution that every 1ml contains 60 μ g, promptly.
The preparation of need testing solution: get content under the content uniformity item, porphyrize is got 0.3g, and accurate the title decides, put in the tool plug conical flask, the accurate 70% ethanol 50ml that adds claims to decide weight, supersound process 30 minutes is put coldly, claims to decide weight again, supply the weight that subtracts mistake with 70% ethanol, shake up, filter, the accurate filtrate 5ml that draws to the 10ml measuring bottle, adds 70% ethanol to scale, shake up, filter, promptly.
Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly.
Every of this product contains Radix Scutellariae with baicalin (C
21H
18O
11) meter, must not be less than 4.5mg.
Claims (9)
1. pharmaceutical composition for the treatment of acne and eczema is characterized in that this pharmaceutical composition is to be made by following raw material medicaments in part by weight:
Flos Lonicerae 40-60 weight portion Herba Taraxaci 40-60 weight portion
Caulis Clematidis Armandii 180-220 weight portion Radix Rehmanniae 120-160 weight portion
Radix Scutellariae 120-160 weight portion Radix Scrophulariae 80-120 weight portion
Cortex Phellodendri 40-60 weight portion Radix Et Rhizoma Rhei 80-120 weight portion
Fel Sus domestica 10-20 weight portion Margarita layer powder 2-5 weight portion
Cornu Saigae Tataricae powder 0.5-2 weight portion Pulvis Cornus Bubali Concentratus 8-12 weight portion.
2. pharmaceutical composition as claimed in claim 1 is characterized in that this pharmaceutical composition is to be made by following raw material medicaments in part by weight:
Flos Lonicerae 50 weight portion Herba Taraxacis 50 weight portion Caulis Clematidis Armandiis 200 weight portions
Radix Rehmanniae 150 weight portion Radix Scutellariaes 150 weight portion Radix Scrophulariaes 100 weight portions
Cortex Phellodendri 50 weight portion Radix et Rhizoma Rhei (parched with wine) 100 weight portion Fel Sus domestica 15 weight portions
Margarita layer powder 3 weight portion Cornu Saigae Tataricae powders 1 weight portion Pulvis Cornus Bubali Concentratus 10 weight portions.
3. pharmaceutical composition as claimed in claim 1 or 2 is characterized in that said composition makes capsule, granule or oral liquid.
4. the preparation method of drug combination preparation as claimed in claim 1 or 2, it is characterized in that this method may further comprise the steps: the Radix Scutellariae of extracting honeysuckle, Herba Taraxaci, Caulis Clematidis Armandii, Radix Rehmanniae, 2/3 weight portion, Radix Scrophulariae, Cortex Phellodendri, Radix Et Rhizoma Rhei add up pharmaceutical composition weight 8-12 decocting doubly and boil 2-4 time, filter, merging filtrate, add Fel Sus domestica and stir evenly, be condensed into thick paste, drying, be ground into fine powder A, standby; The Radix Scutellariae powder of residue 1/3 weight portion is broken into fine powder B, with fine powder A, fine powder B, Margarita layer powder, Cornu Saigae Tataricae powder, Pulvis Cornus Bubali Concentratus mixing; Add conventional adjuvant granulation or encapsulated.
5. the method for quality control of pharmaceutical composition as claimed in claim 3 is characterized in that discrimination method in this method comprises one or more in the following discriminating:
A, get agent of this medicament composition capsule or granule day taking dose 5/9, described every day, dose was equivalent to primary dose 8.646-14.148g; Add methanol 20-40ml supersound process 10-20 minute, filter, filtrate evaporate to dryness, residue add water 15-25ml makes dissolving; Regulating pH value with hydrochloric acid is 1～2, adds ethyl acetate extraction 1-3 time, and each 20-40ml merges ethyl acetate liquid, water 10-20ml washing, and evaporate to dryness, residue add dehydrated alcohol 1ml makes dissolving, as need testing solution; Other gets the baicalin reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw each 5 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with 5-8: 2-4: ethyl acetate-butanone of 1: 1-formic acid-water is developing solvent, pre-equilibration 20-40 minute, launch, take out, dry, spray is with in 1-3% ferric chloride alcoholic solution, the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
B, get Radix Et Rhizoma Rhei control medicinal material 0.1g, add methanol 15-25ml dipping 0.5-1.5 hour, filter, get filtrate 3-7ml, evaporate to dryness, residue add water 8-12ml makes dissolving, add hydrochloric acid 1ml again, put in the water-bath and heated 20-40 minute, immediately cooling, add diethyl ether and extract 1-3 time, each 15-25ml merges ether solution, evaporate to dryness, residue adds dehydrated alcohol 1ml makes dissolving, in contrast medical material solution; Other gets the emodin reference substance, adds dehydrated alcohol and makes the solution that every 1ml contains 0.5mg, in contrast product solution; Test according to thin layer chromatography, draw need testing solution and each 5 μ l of above-mentioned two kinds of solution of differentiating under the B item, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with 5-7: 2: 0.1 normal hexane one ethyl acetate one formic acid is developing solvent, launch, take out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show identical orange-yellow fluorescence principal spot: with the corresponding position of reference substance chromatograph on, show identical orange-yellow fluorescence speckle, put in the ammonia smoked after, inspect under the daylight, speckle becomes redness;
C, get agent of this medicament composition capsule or granule day taking dose 5/9, described every day, dose was equivalent to primary dose 8.646-14.148g; Add methanol 20-40ml, supersound process 10-20 minute, filter, the filtrate evaporate to dryness. residue adds water 15-25ml makes dissolving, extracts the extracting solution evaporate to dryness with water saturated n-butyl alcohol 20-40ml, residue adds methanol 1ml makes dissolving, adds neutral alumina 1g, mixes thoroughly in water-bath, drying is added on 100～200 purpose neutral alumina posts, with ethanol 40-60ml eluting, collect eluent, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution; Other gets Cortex Phellodendri control medicinal material 0.1g, shines medical material solution in pairs with legal system; Get the berberine hydrochloride reference substance again, add methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution; According to thin layer chromatography test, draw each 1 μ l of above-mentioned three kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with 6-8: n-butyl alcohol-glacial acetic acid of 1: 2-water is developing solvent, launches, and takes out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show identical yellow fluorescence speckle;
D, get the peoniflorin reference substance, add methanol and make the solution that every 1ml contains 2mg, in contrast product solution; Test according to thin layer chromatography, prepare need testing solution with reference to the B item, prepare reference substance solution with reference to the C item, draw respectively 4 μ l of need testing solution and reference substance solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with 38-43: 5: 9-12: chloroform-ethyl acetate of 0.2-methanol-formic acid is developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical bluish violet speckle.
6. the method for quality control of pharmaceutical composition as claimed in claim 3 is characterized in that discrimination method in this method comprises one or more in the following discriminating:
A, get agent of this medicament composition capsule or granule day taking dose 5/9, described every day, dose was equivalent to primary dose 8.646-14.148g; Add methanol 30ml supersound process 15 minutes, filter, filtrate evaporate to dryness, residue add water 20ml makes dissolving, regulating pH value with hydrochloric acid is 1～2, adds ethyl acetate extraction 2 times, and each 30ml merges ethyl acetate liquid, water 15ml washing, evaporate to dryness, residue add dehydrated alcohol 1ml makes dissolving, as need testing solution; Other gets the baicalin reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw each 5 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive, with the sodium carboxymethyl cellulose with 6: 3: 1: ethyl acetate-butanone of 1-formic acid-water is developing solvent, pre-equilibration 30 minutes, launch, take out, dry, spray is with in 2% ferric chloride alcoholic solution, the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
B, get Radix Et Rhizoma Rhei control medicinal material 0.1g, add methanol 20ml dipping 1 hour, filter, get filtrate 5ml, evaporate to dryness, residue add water 10ml makes dissolving, add hydrochloric acid 1ml again, put in the water-bath and heated 30 minutes, immediately cooling, add diethyl ether and extract 2 times, each 20ml merges ether solution, evaporate to dryness, residue adds dehydrated alcohol 1ml makes dissolving, in contrast medical material solution; Other gets the emodin reference substance, adds dehydrated alcohol and makes the solution that every 1ml contains 0.5mg, in contrast product solution; Test according to thin layer chromatography, draw need testing solution and each 5 μ l of above-mentioned two kinds of solution of differentiating under the B item, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with 6: 2: 0.1 normal hexane, one ethyl acetate, one formic acid is developing solvent, launch, take out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show identical orange-yellow fluorescence principal spot: with the corresponding position of reference substance chromatograph on, show identical orange-yellow fluorescence speckle, put in the ammonia smoked after, inspect under the daylight, speckle becomes redness;
C, get agent of this medicament composition capsule or granule day taking dose 5/9, described every day, dose was equivalent to primary dose 8.646-14.148g; Add methanol 30ml, supersound process 15 minutes filters, the filtrate evaporate to dryness. residue adds water 20ml makes dissolving, extracts the extracting solution evaporate to dryness with water saturated n-butyl alcohol 30ml, residue adds methanol 1ml makes dissolving, adds neutral alumina 1g, mixes thoroughly in water-bath, drying is added in 100～200 orders, 3g, on the neutral alumina post of internal diameter 1cm,, collect eluent with ethanol 50ml eluting, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution; Other gets Cortex Phellodendri control medicinal material 0.1g, shines medical material solution in pairs with legal system; Get the berberine hydrochloride reference substance again, add methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution; According to thin layer chromatography test, draw each 1 μ l of above-mentioned three kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with n-butyl alcohol-glacial acetic acid of 7: 1: 2-water is developing solvent, launches, and takes out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show identical yellow fluorescence speckle;
D, get the peoniflorin reference substance, add methanol and make the solution that every 1ml contains 2mg, in contrast product solution; Test according to thin layer chromatography, prepare need testing solution with reference to the B item, prepare reference substance solution with reference to the C item, draw respectively 4 μ l of need testing solution and reference substance solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with 40: 5: 10: chloroform-ethyl acetate of 0.2-methanol-formic acid was developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical bluish violet speckle.
7. the method for quality control of pharmaceutical composition as claimed in claim 3 is characterized in that the assay in this method comprises following method:
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; With 40-45: 55-60: 0.2 methanol-water-phosphoric acid is a mobile phase: the detection wavelength is 280nm, and number of theoretical plate calculates by the baicalin peak and is not less than 2000;
The preparation of reference substance solution: it is an amount of that precision takes by weighing the baicalin reference substance, adds methanol and make the solution that every 1ml contains 60 μ g, promptly;
The preparation of need testing solution: get the content of agent of this medicament composition capsule or granule, porphyrize is got 0.2-0.4g, and accurate the title decides, put in the tool plug conical flask, the accurate 60-80% ethanol 45-55ml that adds claims to decide weight, supersound process 20-40 minute, put coldly, claim to decide weight again, supply the weight that subtracts mistake with 60-80% ethanol, shake up, filter, the accurate filtrate 5ml that draws to the 10ml measuring bottle, adds 60-80% ethanol to scale, shake up, filter, promptly;
Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly;
Agent of this medicament composition capsule or granule be the taking dose meter per diem, contains Radix Scutellariae with baicalin C
21H
18O
11Must not be less than 54mg; Described every day, dose was equivalent to primary dose 8.646-14.148g.
8. the method for quality control of pharmaceutical composition as claimed in claim 7 is characterized in that the assay in this method is:
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; With 42: 58: 0.2 methanol-water-phosphoric acid was mobile phase: the detection wavelength is 280nm, and number of theoretical plate calculates by the baicalin peak and is not less than 2000;
The preparation of reference substance solution: it is an amount of that precision takes by weighing the baicalin reference substance, adds methanol and make the solution that every 1ml contains 60 μ g, promptly;
The preparation of need testing solution: get agent of this medicament composition capsule or granule content, porphyrize is got 0.3g, and accurate the title decides, put in the tool plug conical flask, the accurate 70% ethanol 50ml that adds claims to decide weight, supersound process 30 minutes is put coldly, claims to decide weight again, supply the weight that subtracts mistake with 70% ethanol, shake up, filter, the accurate filtrate 5ml that draws to the 10ml measuring bottle, adds 70% ethanol to scale, shake up, filter, promptly;
Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly;
Agent of this medicament composition capsule or granule be the taking dose meter per diem, contains Radix Scutellariae with baicalin C
21H
18O
11Must not be less than 54mg; Described every day, dose was equivalent to primary dose 8.646-14.148g.
9. the application of pharmaceutical composition as claimed in claim 1 or 2 in the medicine of preparation treatment acne and eczema.
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| CNB2005100870072A CN100404047C (en) | 2005-07-22 | 2005-07-22 | Medicinal composition for treating acne and eczema and its preparing method |
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| CN100404047C true CN100404047C (en) | 2008-07-23 |
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| WO2019113805A1 (en) * | 2017-12-12 | 2019-06-20 | 国药集团德众（佛山）药业有限公司 | Acne treatment composition and preparation method therefor |
Citations (3)
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| CN1050519C (en) * | 1995-12-14 | 2000-03-22 | 祝继兴 | Chinese medicine granule for acne |
| CN1368194A (en) * | 2001-02-01 | 2002-09-11 | 杨孟君 | Nano medicine 'Compound Zhenzhu Anchuan' and its praparing process |
| CN1559450A (en) * | 2004-03-05 | 2005-01-05 | 北京建昊嘉信科技有限公司 | Licorice root compound for treating acne |
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2005
- 2005-07-22 CN CNB2005100870072A patent/CN100404047C/en not_active Expired - Fee Related
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|---|---|---|---|---|
| CN1050519C (en) * | 1995-12-14 | 2000-03-22 | 祝继兴 | Chinese medicine granule for acne |
| CN1368194A (en) * | 2001-02-01 | 2002-09-11 | 杨孟君 | Nano medicine 'Compound Zhenzhu Anchuan' and its praparing process |
| CN1559450A (en) * | 2004-03-05 | 2005-01-05 | 北京建昊嘉信科技有限公司 | Licorice root compound for treating acne |
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| 《中华人民共和国卫生部》药品标准（中药成方制剂）第九册. 中华人民共和国卫生部药典委员会，133页，中华人民共和国卫生部. 1994 * |
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