CN100473987C - Quality control method for Chinese medicine composition preparation for treating children's cold - Google Patents
Quality control method for Chinese medicine composition preparation for treating children's cold Download PDFInfo
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- CN100473987C CN100473987C CNB2005101032975A CN200510103297A CN100473987C CN 100473987 C CN100473987 C CN 100473987C CN B2005101032975 A CNB2005101032975 A CN B2005101032975A CN 200510103297 A CN200510103297 A CN 200510103297A CN 100473987 C CN100473987 C CN 100473987C
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Abstract
The present invention discloses a quality control method of Chinese medicine composition for curing infantile common cold. Said method adopts thin-layer chromatography to identify active effective components of scutellaria root, arctium seed, gardenia fruit and forsythia fruit, and utilizes high-performance liquid determination method to determine the content of baicalin.
Description
Technical field
The present invention relates to a kind of method of quality control of Chinese medicinal composition preparation, particularly relate to a kind of method of quality control for the treatment of the Chinese medicinal composition preparation of cold in children.
Background technology
Because children's's internal organs are tender and lovely, taste are strong, and susceptible ailment said due to cold or exposure, cold in children are one of the highest outer perceptual diseases of infant's incidence of disease in period, all can fall ill winter, spring, the outstanding height of morbidity in autumn throughout the year.Easily influence taste digestion and absorption function after the morbidity again, the dry up that stops eating occurs, this sick clinical manifestation is with fever with chilliness, and the cough runny nose sneezes that to wait be cardinal symptom, and the wean to pacify common cold in children particle has effect preferably to treating this disease.Evacuate part of the body cavity above the diaphragm housing the heart and lungs wind-heat based on honeysuckle, the capsule of weeping forsythia; Be aided with the peppermint relieving the exterior syndrome with drugs pungent in flavor and cool in property, the reed rhizome clearing heat and promoting fluid, root of large-flowered skullcap removing heat from the lung to relieve cough, cape jasmine loose heat symptoms caused by an exopathgen and relieving restlessness, the respectful lung of the root of purple-flowered peucedanum reduces phlegm, burdock detoxifcation relieve sore throat, balloonflower root is ventilatingd the lung and resolving phlegm: assistant is with Medicated Leaven, hawthorn, Fructus Hordei Germinatus promoting digestion.In the agent of the hot cold of group's bitter cold, be equipped with ching-chieh, the root of Dahurain angelica that Xin Wen disperses again, the almond of bitter temperature cough-relieving, both increased the power of inducing diaphoresis to dispel wind, and can prevent too cold and cool again and hinder the body of the young sun of children's, all medicines share, be total to the diffusing wind-heat of long memorial, clearing and antitussive, the merit of promoting digestion is for the cold, fever of children's in spring, autumn, generation in winter, sweating is not well, the nasal obstruction runny nose, diseases such as cough pharyngalgia, the curative effect of using is better.The present method of quality control of wean to pacify common cold in children particle comes with some shortcomings, and is difficult to said preparation is carried out more effective quality control.
Summary of the invention
The object of the invention is to provide a kind of method of quality control for the treatment of the Chinese medicinal composition preparation of cold in children.
Technical scheme
The Chinese medicinal composition preparation of treatment cold in children of the present invention is made up of following raw material medicaments, proportioning following (by weight):
Peppermint 50-100 weight portion ching-chieh 40-90 weight portion semen armeniacae amarae 50-100 weight portion
Great burdock achene 50-100 weight portion root of large-flowered skullcap 50-100 weight portion balloonflower root 40-90 weight portion
Root of purple-flowered peucedanum 50-100 weight portion root of Dahurain angelica 10-50 weight portion cape jasmine (stir-fry) 20-60 weight portion
Hawthorn (Jiao) 10-50 weight portion Medicated Leaven (Jiao) 10-50 weight portion Fructus Hordei Germinatus (Jiao) 10-50 weight portion
Reed rhizome 90-150 weight portion honeysuckle 90-150 weight portion capsule of weeping forsythia 50-100 weight portion.
Above-mentioned composition can be made various clinical formulations according to the pharmacy conventional method, as pill, tablet, dripping pill, emulsion, masticatory, oral liquid, capsule, granule etc.
Wherein granule can be prepared as follows: remove peppermint, extracting volatile oil from schizonepeta spike, semen armeniacae amarae is produced outside the almond juice, 12 flavor boilings such as all the other great burdock achenes 2-4 time, each 1-3 hour, filter merging filtrate, left standstill 30-50 hour, and got supernatant concentration to relative density and be 1.30 clear cream, add almond juice, stir evenly, adding sucrose is an amount of, mixing, make particle, drying sprays into above-mentioned volatile oil, promptly.
Method of quality control of the present invention is at by peppermint 50-100 weight portion, ching-chieh 40-90 weight portion, semen armeniacae amarae 50-100 weight portion, great burdock achene 50-100 weight portion, root of large-flowered skullcap 50-100 weight portion, balloonflower root 40-90 weight portion, root of purple-flowered peucedanum 50-100 weight portion, root of Dahurain angelica 10-50 weight portion, cape jasmine (stir-fry) 20-60 weight portion, hawthorn (Jiao) 10-50 weight portion, Medicated Leaven (Jiao) 10-50 weight portion, Fructus Hordei Germinatus (Jiao) 10-50 weight portion, reed rhizome 90-150 weight portion, honeysuckle 90-150 weight portion, capsule of weeping forsythia 50-100 weight portion is the various Chinese medicine preparations that raw material is made, below choose granule and describe, test sample was converted into the dosage suitable with the granule bulk drug when other formulations were used.
Method of quality control of the present invention comprises following discriminating and/or content assaying method.
Discrimination method comprises one or more in the following method:
A. get this product 20g, add water 20ml heating and make dissolving, put coldly, add ethyl acetate and extract 1-3 time, each 30ml, merging ethyl acetate liquid, evaporate to dryness, residue add absolute ethyl alcohol 1ml makes dissolving, as need testing solution; Other gets the scutelloside reference substance, adds methyl alcohol and makes the solution that every 1ml contains 2mg, in contrast product solution; Draw each 3 μ l of above-mentioned two kinds of solution according to thin-layered chromatography, put respectively in same be on the silica gel g thin-layer plate of bonding agent with the sodium carboxymethyl cellulose, ethyl acetate-butanone-formic acid-water with 4-8:-4:1-2:1-2 is developping agent, pre-equilibration 20-40 minute, launch, take out, dry, spray is with 2% ferric trichloride ethanolic solution; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color;
B. get this product 10g, add water 20ml heating and make dissolving, put cold, extract with water saturated normal butyl alcohol 30ml, extract evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, add neutral alumina 1g, in water-bath, mix thoroughly, drying, be added in 100～200 orders, 3g is on the internal diameter 1cm neutral alumina post, with 35-50% methyl alcohol 50ml wash-out, collect eluent, evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as need testing solution; Other gets great burdock achene control medicinal material 0.5g, adds water 20ml reflux 1 hour, filters, and the normal butyl alcohol that filtrate water is saturated shines medicinal material solution in pairs with legal system; According to thin-layered chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be the silica G F of bonding agent with the sodium carboxymethyl cellulose
254On the thin layer plate, be developping agent, launch, take out, dry, put under the 254nm ultraviolet lamp and inspect with the 15-25:1-2 chloroform-methanol, in the test sample chromatogram, with the corresponding position of control medicinal material chromatogram principal spot on, show the spot of same color;
C. get this product 10g, add water 20ml heating and make dissolving, put cold, extract with water saturated normal butyl alcohol 30ml, extract evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, add neutral alumina 1g, in water-bath, mix thoroughly, drying, be added in 100～200 orders, 3g is on the internal diameter 1cm neutral alumina post, with 35-50% methyl alcohol 50ml wash-out, collect eluent, evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as need testing solution; Get the Gardenoside reference substance, add methyl alcohol and make the solution that every 1ml contains 2mg, in contrast product solution; Test according to thin-layered chromatography, draw each 5 μ l of need testing solution and above-mentioned reference substance solution, put respectively in same be on the silica gel g thin-layer plate of bonding agent with the sodium carboxymethyl cellulose, with the 3-5:1-2 chloroform-methanol is developping agent, launch, take out, dry, spray is with the 8-12% ethanol solution of sulfuric acid, and 100-110 ℃ to be heated to the spot colour developing clear; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color;
D. get this product 10g, add water 20ml heating and make dissolving, put cold, extract with water saturated normal butyl alcohol 30ml, extract evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, add neutral alumina 1g, in water-bath, mix thoroughly, drying, be added in 100～200 orders, 3g is on the internal diameter 1cm neutral alumina post, with 35-50% methyl alcohol 50ml wash-out, collect eluent, evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as need testing solution; Get capsule of weeping forsythia control medicinal material 0.8g, add water 20ml reflux 0.5-1.5 hour, filter, the normal butyl alcohol 30ml that filtrate water is saturated extracts, and extract evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, add neutral alumina 1g, in water-bath, mix thoroughly, drying, be added in 100～200 orders, 3g is on the internal diameter 1cm neutral alumina post, with 35-50% methyl alcohol 50ml wash-out, collect eluent, evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, makes control medicinal material solution; Test according to thin-layered chromatography, draw each 10 μ l of need testing solution and above-mentioned control medicinal material solution, put respectively in same be on the silica gel g thin-layer plate of bonding agent with the sodium carboxymethyl cellulose, with 7-9:10-13:1-2 normal hexane-chloroform-methanol is developping agent, launch, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear to be heated to the spot colour developing; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram principal spot on, show the spot of same color;
Assay:
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filling agent; With the 40-50:50-60:0.1-0.4 methanol-water-phosphoric acid is moving phase; The detection wavelength is 280nm, and number of theoretical plate calculates by the scutelloside peak and is not less than 2500; The preparation of reference substance solution: it is an amount of that precision takes by weighing the scutelloside reference substance, adds methyl alcohol and make the solution that every 1ml contains 60 μ g, promptly; This product under the weight differential item is got in the preparation of need testing solution, gets 1g, and accurate the title decides, and puts in the tool plug conical flask, the accurate 60-80% ethanol 50ml that adds claims decide weight, and sonicated 25-35 minute, put coldly, weight decided in title again, supply the weight that subtracts mistake with 65-75% ethanol, shake up, filter, promptly; Determination method, accurate respectively reference substance solution and each 10ul of need testing solution of drawing injects liquid chromatograph, measures, promptly.
By discovering, when in the discriminating of method of quality control, selecting peppermint, schizonepeta and honeysuckle as the medicinal material differentiated, poor effect, and method of quality control of the present invention is by the screening to each medicinal material, the discriminating medicinal material of selecting and as the composition of assay, can reach effective control, and, make method precision, sensitivity, stability all higher by to each method screening to the quality of product.
Following experiment and embodiment are used to further specify but are not limited to the present invention.
Experimental example 1Assay research
1, instrument and reagent
SP8810 high performance liquid chromatograph: Spectra 100 UV-detector; SP4270 integraph: SEPU3000P workstation: Unicam Uv530 ultraviolet-visible pectrophotometer; KQ-i00 type ultrasonic cleaner.Scutelloside reference substance (715-200111 is for assay Nat'l Pharmaceutical ﹠ Biological Products Control Institute).Methyl alcohol: chromatographically pure: water: ultrapure water: other reagent: it is pure to be analysis,
2, high-efficient liquid phase chromatogram condition:
The stainless steel column of Ilypersil ODS2 (4.6 * 200mm, 5 μ m); Moving phase: methanol-water-phosphoric acid (44:56:0.2); Flow velocity: 1.0ml/min; Detect ripple K:280nm; Column temperature: room temperature.
3, typical curve
It is an amount of that precision takes by weighing the scutelloside reference substance, adds methyl alcohol and make the solution that every 1ml contains scutelloside 30.4,60.8,91.2,121.6,152.0 μ g.Draw 10 μ l respectively, press content assaying method and measure peak area.The results are shown in Table 1.
Table 1
As ordinate, X is as abscissa for reference substance concentration, carries out linear regression with the peak area Y that records, linear equation y=24940X+59787; R=0.9996; The range of linearity 30.4～152.0 μ g.
4, the preparation of need testing solution
" extracting method under " root of large-flowered skullcap " assay of Chinese pharmacopoeia version in 2000 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 lotion is filtered in the same measuring bottle, add 70% ethanol to scale, shake up.The accurate 1ml that draws to the 10ml measuring bottle, adds 70% ethanol to scale, shakes up, promptly.
The root of large-flowered skullcap in this product prescription is an extraction process by water.For investigating the preparation condition of need testing solution, with reference to above-mentioned preparation method, get this product 1g respectively, the accurate title, decide, and as extracting solvent, tests as follows with 70% ethanol:
1. press the preparation method of embodiment 1, ultrasonic 20 minutes, 30 minutes, 60 minutes respectively, make need testing solution A, B, C.
2. the accurate 70% ethanol 50ml that adds claims decide weight, and reflux 1 hour is put coldly, claims to decide weight again, supplies the weight that subtracts mistake with 70% ethanol, shake up, and filtration, filtrate is as need testing solution D.
Draw each 10 μ l of above-mentioned need testing solution respectively, press content assaying method and measure the sweet content of the root of large-flowered skullcap, the results are shown in Table 2.
Table 2
Because this product adds 70% ethanol sonicated, this product can be disperseed fully above disposal route, test findings content is basic identical, all the scutelloside in the sample can be extracted fully, in conjunction with application of sample recovery test result, select sonicated 30 minutes, as the preparation method of need testing solution.
5, the preparation of reference substance solution
It is an amount of that precision takes by weighing the scutelloside reference substance, adds methyl alcohol and make the solution that every 1ml contains 60 μ g, promptly.In the official method, get reference substance 60 ℃ of drying under reduced pressure weighings after 4 hours.Through test, get above-mentioned test sample (assay is used), after the official method drying, weight does not have change, directly weighing.
6, determination method
The selection of moving phase: " moving phase under " root of large-flowered skullcap " assay of Chinese pharmacopoeia version in 2000 item is methanol-water-phosphoric acid (47:53:0.2), through suitable proportioning, the ratio of moving phase is with methanol-water-phosphoric acid (44:56:0.2), and scutelloside peak and adjacent peak degree of separation are better.
7, blank test
Get the scarce root of large-flowered skullcap negative sample 1g in prescription ratio and method for making preparation, handle and measure by the preparation and the assay method of need testing solution, the result does not see that blank test has interference.
8, precision test
The above-mentioned scutelloside reference substance solution 10 μ l of accurate absorption press content assaying method and repeat sample introduction 5 times, measure the absorption peak area.The results are shown in Table 3.
Table 3:
9, replica test
Get same test sample (lot number: 20040801), porphyrize, precision takes by weighing 5 parts, presses content assaying method and measures.The results are shown in Table 4.
Table 4:
10, stability test
The same need testing solution of accurate absorption after start was waited to stablize in 1 hour, at 0,2,4,6,8 and 12 hour, injects high performance liquid chromatograph respectively, presses content assaying method and measures peak area.The results are shown in Table 5.
Table 5
11, application of sample recovery test
Get test sample (lot number: 20040801: contain scutelloside 3.5759mg/g) porphyrize, get 5 parts of each 1g, the accurate title, decide, accurate scutelloside reference substance solution (3.20mg/ml) 1ml that adds, water-bath volatilizes, and measures by the above-mentioned content assaying method of drafting, and the results are shown in Table 6.
Table 6
12, sample size is measured
Get 3 batches of this product, measure, with content of baicalin in the external standard method calculation sample by method under the assay item.The results are shown in Table 7.
Table 7
According to above-mentioned test findings,, order every bag of this product temporarily and contain the root of large-flowered skullcap with scutelloside (C with 80% calculating
21H
18O
11) meter, must not be less than 28.0mg.
Following embodiment all can realize the effect of above-mentioned experimental example.
Embodiment 1:
Peppermint 80g ching-chieh 67g semen armeniacae amarae 80g great burdock achene 80g
Root of large-flowered skullcap 80g balloonflower root 67g root of purple-flowered peucedanum 80g root of Dahurain angelica 27g
Cape jasmine (stir-fry) 40g hawthorn (Jiao) 27g Medicated Leaven (Jiao) 27g Fructus Hordei Germinatus (Jiao) 27g
Reed rhizome 120g honeysuckle 120g capsule of weeping forsythia 80g
(method for making) above ten five tastes remove peppermint, extracting volatile oil from schizonepeta spike, and semen armeniacae amarae is produced outside the almond juice, 12 flavor boiling secondaries such as all the other great burdock achenes, 2 hours for the first time, 1 hour for the second time, filter merging filtrate, left standstill 48 hours, and got supernatant concentration to relative density and be 1.30 clear cream, add almond juice, stir evenly, adding sucrose is an amount of, mixing, make particle, drying sprays into above-mentioned volatile oil, mixing is distributed into 100 bags, promptly.
Method of quality control:
Differentiate:
A. get this product 20g, add water 20ml heating and make dissolving, put coldly, add ethyl acetate and extract 2 times, each 30ml merges ethyl acetate liquid, and evaporate to dryness, residue add absolute ethyl alcohol 1ml makes dissolving, as need testing solution.Other gets the scutelloside reference substance, adds methyl alcohol and makes the solution that every 1ml contains 2mg, in contrast product solution.Test according to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B), draw each 3 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, with ethyl acetate-butanone-formic acid-water (6:3:1:1) is developping agent, pre-equilibration 30 minutes launches, and takes out, dry, spray is with 2% ferric trichloride ethanolic solution.In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color.
B. get this product 10g, add water 20ml heating and make dissolving, put cold, extract with water saturated normal butyl alcohol 30ml, extract evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, add neutral alumina 1g, in water-bath, mix thoroughly, drying, be added on the neutral alumina post (100～200 orders, 3g, internal diameter 1cm), with 40% methyl alcohol 50ml wash-out, collect eluent, evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as need testing solution.Other gets great burdock achene control medicinal material 0.5g, adds water 20ml reflux 1 hour, filters, and the normal butyl alcohol that filtrate water is saturated shines medicinal material solution in pairs with legal system.According to thin-layered chromatography (China about allusion quotation version in 2000 an appendix VI B) test, draw respectively 10 μ l of above-mentioned two kinds of solution, put respectively in same be the silica G F of binder with the sodium carboxymethyl cellulose
254On the thin layer plate, be developping agent, launch, take out, dry, put under the ultraviolet lamp (254nm) and inspect with chloroform-methanol (20:1), in the test sample chromatogram, with the corresponding position of control medicinal material chromatogram principal spot on, show the spot of same color.
Embodiment 2:
Wean to pacify common cold in children granular mass control method: (raw material composition and method for making are with embodiment 1)
Differentiate:
A. get this product 20g, add water 20ml heating and make dissolving, put coldly, add ethyl acetate and extract 2 times, each 30ml merges ethyl acetate liquid, and evaporate to dryness, residue add absolute ethyl alcohol 1ml makes dissolving, as need testing solution.Other gets the scutelloside reference substance, adds methyl alcohol and makes the solution that every 1ml contains 2mg, in contrast product solution.Test according to thin-layered chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000), draw each 3 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, with ethyl acetate-butanone-formic acid-water (6:3:1:1) is developping agent, pre-equilibration 30 minutes launches, and takes out, dry, spray is with 2% ferric trichloride ethanolic solution.In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color.
B. get this product 10g, add water 20ml heating and make dissolving, put cold, extract with water saturated normal butyl alcohol 30ml, extract evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, add neutral alumina 1g, in water-bath, mix thoroughly, drying, be added on the neutral alumina post (100～200 orders, 3g, internal diameter 1cm), with 40% methyl alcohol 50ml wash-out, collect eluent, evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as need testing solution.Other gets great burdock achene control medicinal material 0.5g, adds water 20ml reflux 1 hour, filters, and the normal butyl alcohol that filtrate water is saturated shines medicinal material solution in pairs with legal system.According to thin-layered chromatography (China about allusion quotation version in 2000 an appendix VI B) test, draw respectively 10 μ l of above-mentioned two kinds of solution, put respectively in same be the silica G F of binder with the sodium carboxymethyl cellulose
254On the thin layer plate, be developping agent, launch, take out, dry, put under the ultraviolet lamp (254nm) and inspect with chloroform-methanol (20:1), in the test sample chromatogram, with the corresponding position of control medicinal material chromatogram principal spot on, show the spot of same color.
C. get this product 10g, add water 20ml heating and make dissolving, put cold, extract with water saturated normal butyl alcohol 30ml, extract evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, add neutral alumina 1g, in water-bath, mix thoroughly, drying, be added on the neutral alumina post (100～200 orders, 3g, internal diameter 1cm), with 40% methyl alcohol 50ml wash-out, collect eluent, evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as need testing solution.Get the Gardenoside reference substance, add methyl alcohol and make the solution that every 1ml contains 2mg, in contrast product solution.Test according to thin-layered chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000), draw each 5 μ l of need testing solution and above-mentioned reference substance solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, with chloroform-methanol (4:1) is developping agent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and 105 ℃ to be heated to the spot colour developing clear.In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color.
D. get this product 10g, add water 20ml heating and make dissolving, put cold, extract with water saturated normal butyl alcohol 30ml, extract evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, add neutral alumina 1g, in water-bath, mix thoroughly, drying, be added on the neutral alumina post (100～200 orders, 3g, internal diameter 1cm), with 40% methyl alcohol 50ml wash-out, collect eluent, evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as need testing solution.Get capsule of weeping forsythia control medicinal material 0.8g, add water 20ml reflux 1 hour, filter, the saturated normal butyl alcohol of filtrate water is made control medicinal material solution with the preparation method of above-mentioned need testing solution.Test according to thin-layered chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000), draw each 10 μ l of need testing solution and above-mentioned control medicinal material solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, with normal hexane-chloroform-methanol (8:11:1) is developping agent, launch, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear to be heated to the spot colour developing.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram principal spot on, show the spot of same color.
Assay:
According to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2000).
Chromatographic condition and system suitability test octadecylsilane chemically bonded silica are filling agent; With methanol-water-phosphoric acid (44:56:0.2) is moving phase; The detection wavelength is 280nm, and number of theoretical plate calculates by the scutelloside peak and is not less than 2500.
The preparation of reference substance solution: it is an amount of that precision takes by weighing the scutelloside reference substance, adds methyl alcohol and make the solution that every 1ml contains 60 μ g, promptly.This product under the weight differential item is got in the preparation of need testing solution, gets 1g, and accurate the title decides, and puts in the tool plug conical flask, the accurate 70% ethanol 50ml that adds, claim decide weight, sonicated 30 minutes is put coldly, and weight decided in title again, supply the weight that subtracts mistake with 70% ethanol, shake up, filter, promptly.Determination method, accurate respectively reference substance solution and each 10ul of need testing solution of drawing injects liquid chromatograph, measures, promptly.This product contains the root of large-flowered skullcap with scutelloside (C for every bag
21H
18O
11) meter, must not be less than 28.0mg.
Claims (3)
1, a kind of method of quality control for the treatment of the Chinese medicinal composition preparation of cold in children is characterized in that this method comprises the steps:
Assay:
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filling agent; With the 40-50:50-60:0.1-0.4 methanol-water-phosphoric acid is moving phase; The detection wavelength is 280nm, and number of theoretical plate calculates by the scutelloside peak and is not less than 2500; The preparation of reference substance solution: it is an amount of that precision takes by weighing the scutelloside reference substance, adds methyl alcohol and make the solution that every 1ml contains 60 μ g, promptly; The preparation of need testing solution: get the composite preparation under the weight differential item, get 1g, the accurate title, decide, put in the tool plug conical flask, the accurate 60-80% ethanol 50ml that adds claims to decide weight, sonicated 25-35 minute, put cold, claim again to decide weight, supply the weight that subtracts mistake, shake up with 65-75% ethanol, filter, promptly; Determination method, accurate respectively reference substance solution and each 10ul of need testing solution of drawing injects liquid chromatograph, measures, promptly;
Differentiate:
A. get composite preparation 20g, add water 20ml heating and make dissolving, put coldly, add ethyl acetate and extract 1-3 time, each 30ml, merging ethyl acetate liquid, evaporate to dryness, residue add absolute ethyl alcohol 1ml makes dissolving, as need testing solution; Other gets the scutelloside reference substance, adds methyl alcohol and makes the solution that every 1ml contains 2mg, in contrast product solution; Draw each 3 μ l of above-mentioned two kinds of solution according to thin-layered chromatography, put respectively in same be on the silica gel g thin-layer plate of bonding agent with the sodium carboxymethyl cellulose, ethyl acetate-butanone-formic acid-water with 4-8:2-4:1-2:1-2 is developping agent, pre-equilibration 20-40 minute, launch, take out, dry, spray is with 2% ferric trichloride ethanolic solution; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color;
B. get composite preparation 10g, add water 20ml heating and make dissolving, put cold, extract with water saturated normal butyl alcohol 30ml, extract evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, add neutral alumina 1g, in water-bath, mix thoroughly, drying, be added in 100～200 orders, 3g is on the internal diameter 1cm neutral alumina post, with 35-50% methyl alcohol 50ml wash-out, collect eluent, evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as need testing solution; Other gets great burdock achene control medicinal material 0.5g, adds water 20ml reflux 1 hour, filters, and the normal butyl alcohol that filtrate water is saturated shines medicinal material solution in pairs with legal system; According to thin-layered chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be the silica G F of bonding agent with the sodium carboxymethyl cellulose
254On the thin layer plate, be developping agent, launch, take out, dry, put under the 254nm ultraviolet lamp and inspect with the 15-25:1-2 chloroform-methanol, in the test sample chromatogram, with the corresponding position of control medicinal material chromatogram principal spot on, show the spot of same color;
C. get composite preparation 10g, add water 20ml heating and make dissolving, put cold, extract with water saturated normal butyl alcohol 30ml, extract evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, add neutral alumina 1g, in water-bath, mix thoroughly, drying, be added in 100～200 orders, 3g is on the internal diameter 1cm neutral alumina post, with 35-50% methyl alcohol 50ml wash-out, collect eluent, evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as need testing solution; Get the Gardenoside reference substance, add methyl alcohol and make the solution that every 1ml contains 2mg, in contrast product solution; Test according to thin-layered chromatography, draw each 5 μ l of need testing solution and above-mentioned reference substance solution, put respectively in same be on the silica gel g thin-layer plate of bonding agent with the sodium carboxymethyl cellulose, with the 3-5:1-2 chloroform-methanol is developping agent, launch, take out, dry, spray is with the 8-12% ethanol solution of sulfuric acid, and 100-110 ℃ to be heated to the spot colour developing clear; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color;
D. get composite preparation 10g, add water 20ml heating and make dissolving, put cold, extract with water saturated normal butyl alcohol 30ml, extract evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, add neutral alumina 1g, in water-bath, mix thoroughly, drying, be added in 100～200 orders, 3g is on the internal diameter 1cm neutral alumina post, with 35-50% methyl alcohol 50ml wash-out, collect eluent, evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as need testing solution; Get capsule of weeping forsythia control medicinal material 0.8g, add water 20ml reflux 0.5-1.5 hour, filter, the normal butyl alcohol 30ml that filtrate water is saturated extracts, and extract evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, add neutral alumina 1g, in water-bath, mix thoroughly, drying, be added in 100～200 orders, 3g is on the internal diameter 1cm neutral alumina post, with 35-50% methyl alcohol 50ml wash-out, collect eluent, evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, makes control medicinal material solution; Test according to thin-layered chromatography, draw each 10 μ l of need testing solution and above-mentioned control medicinal material solution, put respectively in same be on the silica gel g thin-layer plate of bonding agent with the sodium carboxymethyl cellulose, with 7-9:10-13:1-2 normal hexane-chloroform-methanol is developping agent, launch, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear to be heated to the spot colour developing; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram principal spot on, show the spot of same color;
Described composition is by peppermint 50-100 weight portion, ching-chieh 40-90 weight portion, semen armeniacae amarae 50-100 weight portion, great burdock achene 50-100 weight portion, root of large-flowered skullcap 50-100 weight portion, balloonflower root 40-90 weight portion, root of purple-flowered peucedanum 50-100 weight portion, root of Dahurain angelica 10-50 weight portion, stir-baked FRUCTUS GARDENIAE 20-60 weight portion, charred FRUCTUS CRATAEGI 10-50 weight portion, burnt Medicated Leaven 10-50 weight portion, melanoidin malt 10-50 weight portion, reed rhizome 90-150 weight portion, honeysuckle 90-150 weight portion, capsule of weeping forsythia 50-100 weight portion is the various preparations that raw material is made.
2, method of quality control as claimed in claim 1 is characterized in that this method comprises the steps:
Assay:
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filling agent; With the 44:56:0.2 methanol-water-phosphoric acid is moving phase; The detection wavelength is 280nm, and number of theoretical plate calculates by the scutelloside peak and is not less than 2500;
The preparation of reference substance solution: it is an amount of that precision takes by weighing the scutelloside reference substance, adds methyl alcohol and make the solution that every 1ml contains 60 μ g, promptly; The composition grain preparation under the weight differential item is got in the preparation of need testing solution, gets 1g, and accurate the title decides, and puts in the tool plug conical flask, the accurate 70% ethanol 50ml that adds, claim decide weight, sonicated 30 minutes is put coldly, and weight decided in title again, supply the weight that subtracts mistake with 70% ethanol, shake up, filter, promptly; Determination method, accurate respectively reference substance solution and each 10ul of need testing solution of drawing injects liquid chromatograph, measures, promptly;
Differentiate:
A. get composite preparation 20g, add water 20ml heating and make dissolving, put coldly, add ethyl acetate and extract 2 times, each 30ml merges ethyl acetate liquid, and evaporate to dryness, residue add absolute ethyl alcohol 1ml makes dissolving, as need testing solution; Other gets the scutelloside reference substance, adds methyl alcohol and makes the solution that every 1ml contains 2mg, in contrast product solution; Draw each 3 μ l of above-mentioned two kinds of solution according to thin-layered chromatography, put respectively in same be on the silica gel g thin-layer plate of bonding agent with the sodium carboxymethyl cellulose, ethyl acetate-butanone-formic acid-water with 6:3:1:1 is developping agent, pre-equilibration 30 minutes, launch, take out, dry, spray is with 2% ferric trichloride ethanolic solution; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color;
B. get composite preparation 10g, add water 20ml heating and make dissolving, put cold, extract with water saturated normal butyl alcohol 30ml, extract evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, add neutral alumina 1g, in water-bath, mix thoroughly, drying, be added in 100～200 orders, 3g is on the internal diameter 1cm neutral alumina post, with 40% methyl alcohol 50ml wash-out, collect eluent, evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as need testing solution; Other gets great burdock achene control medicinal material 0.5g, adds water 20ml reflux 1 hour, filters, and the normal butyl alcohol that filtrate water is saturated shines medicinal material solution in pairs with legal system; According to thin-layered chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be the silica G F of bonding agent with the sodium carboxymethyl cellulose
254On the thin layer plate, be developping agent, launch, take out, dry, put under the 254nm ultraviolet lamp and inspect with the 20:1 chloroform-methanol, in the test sample chromatogram, with the corresponding position of control medicinal material chromatogram principal spot on, show the spot of same color;
C. get composite preparation 10g, add water 20ml heating and make dissolving, put cold, extract with water saturated normal butyl alcohol 30ml, extract evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, add neutral alumina 1g, in water-bath, mix thoroughly, drying, be added in 100～200 orders, 3g is on the internal diameter 1cm neutral alumina post, with 40% methyl alcohol 50ml wash-out, collect eluent, evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as need testing solution; Get the Gardenoside reference substance, add methyl alcohol and make the solution that every 1ml contains 2mg, in contrast product solution; Test according to thin-layered chromatography, draw each 5 μ l of need testing solution and above-mentioned reference substance solution, put respectively in same be on the silica gel g thin-layer plate of bonding agent with the sodium carboxymethyl cellulose, with the 4:1 chloroform-methanol is developping agent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and 105 ℃ to be heated to the spot colour developing clear; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color;
D. get composite preparation 10g, add water 20ml heating and make dissolving, put cold, extract with water saturated normal butyl alcohol 30ml, extract evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, add neutral alumina 1g, in water-bath, mix thoroughly, drying, be added in 100～200 orders, 3g is on the internal diameter 1cm neutral alumina post, with 40% methyl alcohol 50ml wash-out, collect eluent, evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as need testing solution; Get capsule of weeping forsythia control medicinal material 0.8g, add water 20ml reflux 1 hour, filter, extract with water saturated normal butyl alcohol 30ml, extract evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, add neutral alumina 1g, in water-bath, mix thoroughly, drying, be added in 100～200 orders, 3g is on the internal diameter 1cm neutral alumina post, with 40% methyl alcohol 50ml wash-out, collect eluent, evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, makes control medicinal material solution; Test according to thin-layered chromatography, draw each 10 μ l of need testing solution and above-mentioned control medicinal material solution, put respectively in same be on the silica gel g thin-layer plate of bonding agent with the sodium carboxymethyl cellulose, with 8:11:1 normal hexane-chloroform-methanol is developping agent, launch, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear to be heated to the spot colour developing; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram principal spot on, show the spot of same color;
Described composite preparation is the granule of being made by peppermint 80 weight portions, ching-chieh 67 weight portions, semen armeniacae amarae 80 weight portions, great burdock achene 80 weight portions, the root of large-flowered skullcap 80 weight portions, balloonflower root 67 weight portions, the root of purple-flowered peucedanum 80 weight portions, the root of Dahurain angelica 27 weight portions, stir-baked FRUCTUS GARDENIAE 40 weight portions, charred FRUCTUS CRATAEGI 27 weight portions, burnt Medicated Leaven 27 weight portions, melanoidin malt 27 weight portions, reed rhizome 120 weight portions, honeysuckle 120 weight portions, the capsule of weeping forsythia 80 weight portions.
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| CN104833751B (en) * | 2015-04-28 | 2016-06-29 | 吉林益民堂制药有限公司 | The method for building up of XIAOER GANMAO TANGJIANG Aqueous extracts HPLC standard finger-print and application thereof |
| CN105456834A (en) * | 2016-01-14 | 2016-04-06 | 江西京通美联药业有限公司 | Preparation method of medicine preparation for treating common cold in children |
| CN110187044B (en) * | 2019-01-17 | 2021-04-27 | 山东省农业科学院家禽研究所 | Quality detection method of Yinqiao detoxification oral liquid |
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Non-Patent Citations (5)
| Title |
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| 中华人民共和国***药品标准 中药成方制剂 第9册29页. 29，药典委员会. 1994 中华人民共和国药典2000年版第一部404－405页. 国家药典委员会，404－405，化学工业出版社. 2000 |
| 中华人民共和国***药品标准 中药成方制剂 第9册29页. 29，药典委员会. 1994 * |
| 中华人民共和国药典2000年版第一部404－405页. 国家药典委员会，404－405，化学工业出版社. 2000 * |
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