CN102233097A - Quality control method for Zengguang capsules - Google Patents
Quality control method for Zengguang capsules Download PDFInfo
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- CN102233097A CN102233097A CN2010101650418A CN201010165041A CN102233097A CN 102233097 A CN102233097 A CN 102233097A CN 2010101650418 A CN2010101650418 A CN 2010101650418A CN 201010165041 A CN201010165041 A CN 201010165041A CN 102233097 A CN102233097 A CN 102233097A
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Abstract
The invention provides a new quality control method for Zengguang capsules and overcomes the drawbacks of the prior art. In the invention, the content of ferulic acid in the compound preparation, namely the Zengguang capsules, is measured by high efficiency liquid chromatography; and the thin-layer chromatography identification of medlar, which is the main medicine of the compound preparation, and medicinal materials including Codonopsis pilosula and Schisandra chinensis is performed, so the accuracy and advancement of the quality control method of the compound preparation are ensured, and the product quality of the Zengguang capsules can be controlled more effectively.
Description
Technical field
The present invention relates to the compound Chinese medicinal preparation capsular method of quality control that adds lustre to.
Technical background
Compound Chinese medicinal preparation add lustre to capsule by Chinese crude drug Fructus Lycii 200g, Radix Codonopsis 100g, Radix Angelicae Sinensis 100g, Radix Ophiopogonis 36g, Poria 30g, Rhizoma Alismatis 24g, Cortex Moutan 24g, Fructus Schisandrae Chinensis 18g, Rhizoma Acori Graminei 18g, Radix Polygalae (liquorice beverage system) 18g form, above-mentioned raw materials is made 1000 altogether.Main flavour of a drug in the Fructus Lycii side of being, the dry mature fruit for plant of Solanaceae lycium barbarum Lycium barbarum L. has nourishing the liver and kidney, the effect of replenishing vital essence to improve eyesight; Radix Codonopsis is the dry root of campanulaceae plant Radix Codonopsis Codonopsispilosula (Franch.) Nannf., plain flower Radix Codonopsis Codonopsis pilosula Nannf.var.modesta (Nannf.) L.T.Shen or radix codonpsis tangshen Codonopsis tangshenOliv., has invigorating the spleen and replenishing QI, the effect of spleen invigorating lung benefiting; When the dry root that is classified as umbelliferae angelica Angelica sinensis (Oliv.) Diels, having enriches blood invigorates blood circulation, menstruction regulating and pain relieving, the effect of loosening bowel to relieve constipation; Be the dried root of liliaceous plant Ophiopogon Radix Ophiopogonis japonicus (Thunb.) Ker-Gawl. Radix Ophiopogonis, has YIN nourishing and the production of body fluid promoting, the effect that lung moistening clears away heart-fire; Poria is the dry sclerotia of Polyporaceae fungus Poria Poria cocos (Schw.) Wolf, has promoting diuresis to eliminate damp pathogen, the effect of spleen invigorating mind calming; Rhizoma Alismatis is the dry tuber of Alismataceae plant Rhizoma Alismatis Alismaorientalis (Sam.) Juzep., has diuresis, the effect of clearing away damp-heat; Cortex Moutan is the dry root bark of ranunculaceae peony Paeonia suffruticosa Andr., has clearing away heat and cooling blood, the effect of blood circulation promoting and blood stasis dispelling; Fructus Schisandrae Chinensis is the dry mature fruit of magnoliaceae schisandra Schisandra chinensis (Turcz.) Baill., have the convergence astringent or styptic treatment for spontaneous sweating, supplementing QI for promoting the production of body fluid, the effect of kidney calming; Rhizoma Acori Graminei is the dry rhizome of acorus gramineus araceae plant Acorus tatarinowii Schott, has the removing dampness appetizing, the eliminating phlegm of having one's ideas straightened out, the effect of refreshment Fructus Alpiniae Oxyphyllae; Radix Polygalae is the dry root of milk wort Radix Polygalae Polygalatenuifolia Willd. or ovum leaf Radix Polygalae Polygala sibirica L., has the Fructus Alpiniae Oxyphyllae of calming the nerves, and eliminates the phlegm the effect of detumescence; The ten quality control standard of having issued brightening piece of " Drug Standard of Ministry of Public Health of the Peoples Republic of China " (Chinese traditional patent formulation preparation), this tablet is identical with the capsular prescription that adds lustre to, but have only microscopical identification and physicochemical identification in the method for quality control that its Ministry of Public Health is issued, limitation is very big, is difficult to accurately control drug quality; The present invention has overcome the deficiencies in the prior art, improved the capsular quality control standard of adding lustre to, the assay index and the detection method thereof of said preparation have been set up, increased wherein the principal agent Fructus Lycii and the thin layer chromatography qualitative identification method of medical material Radix Codonopsis, Fructus Schisandrae Chinensis, guaranteed the quality standard level of this compound preparation.The time 2005 the 16th the 12nd phases of volume of precious traditional Chinese medical science traditional Chinese medicines reported the method for content of ferulic acid in the high effective liquid chromatography for measuring brightening piece, there is following defective (1) reflux, extract, energy waste height in this method, processing safety is poor; (2) be to extract solvent with the chloroform, this solvent has intensive liver toxicity, and is harmful to health; (3) repeatability of measurement result is relatively poor.The present invention improves above defective, and methanol with 70% or ethanol serve as to extract solvent supersonic to extract, save the safety of the energy and method and as a result accuracy all be greatly improved.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, formulate the new capsular method of quality control that adds lustre to, by utilizing content of ferulic acid in this compound preparation of high effective liquid chromatography for measuring; The thin layer chromatography that increases principal agent Fructus Lycii in this compound preparation and medical material Radix Codonopsis, Fructus Schisandrae Chinensis differentiates, thereby guaranteed the accuracy and the advance of this compound preparation quality determining method, can control the capsular product quality of adding lustre to more effectively.
The present invention is achieved by following technical proposals:
The quality control detection method that the capsule that adds lustre to is new, this scheme comprises following determination step:
1. measure ferulic acid (C in the capsule that adds lustre to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 D)
18H
21O
3) content:
A. chromatographic condition: with the octadecylsilane chemically bonded silica is filler; (25-35: 65-75) be mobile phase, the detection wavelength is 320 ± 7nm to methanol-0.1% phosphoric acid solution;
B. the preparation of reference substance solution: it is an amount of that precision takes by weighing the ferulic acid reference substance, puts in the brown measuring bottle, adds in methanol or the ethanol any and make the solution that every 1ml contains 5--50 μ g, promptly;
C. the preparation of need testing solution: get the content of this product 2-15 grain, the accurate title, decided mixing, porphyrize is got 0.1-2g, and accurate the title decides, put in the tool plug conical flask, accurate any 10～50ml that adds in 10～100% methanol or the ethanol claims to decide weight, supersound process 0.5-2 hour, put cold, claim to decide weight again, supply the weight that subtracts mistake, shake up with in 10～100% methanol or the ethanol any, filter, precision is measured subsequent filtrate 1-25ml, volatilizes, and residue adds in 10～100% methanol or the ethanol any and is transferred in the 2-10ml measuring bottle, add in 10～100% methanol or the ethanol any to scale, shake up, filter with 0.45 μ m microporous filter membrane, promptly;
D. content of ferulic acid assay method: accurate respectively reference substance solution and each 5--20 μ l of need testing solution of drawing, inject chromatograph of liquid, the mensuration content of ferulic acid;
E. every contains Radix Angelicae Sinensis with ferulic acid (C
18H
21O
3) meter, must not be less than 35 μ g;
The present invention serves as to extract solvent supersonic to extract with 70% methanol or ethanol, than the time precious traditional Chinese medical science traditional Chinese medicines the 12nd phase of 2005 the 16th volumes report the high effective liquid chromatography for measuring brightening piece in the content of ferulic acid method therefor save the safety of the energy and method and as a result accuracy all be greatly improved.Specific as follows:
Test example 1: the capsule content that adds lustre to is measured
Get the capsule finished product that adds lustre to a collection of (lot number 100201), carry out assay by literature method and method of the present invention respectively, the result is as follows:
The result who measures shows that the RSD of the inventive method measurement result (%) value obviously is better than literature method.
2. this medicine Chinese crude drug Radix Codonopsis is differentiated with thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B):
A. the preparation of control medicinal material solution: get Radix Codonopsis control medicinal material 1-5g, add n-butyl alcohol 15-75ml, reflux 1-4 hour, filter, filtrate is reclaimed n-butyl alcohol to 1-5ml, makes control medicinal material solution;
B. the preparation of need testing solution: get this product content 1-5g, add n-butyl alcohol 10-50ml, reflux 1-4 hour, filter, filtrate is reclaimed n-butyl alcohol to 1-5ml, makes need testing solution;
C. test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B): draw each 1-15 μ l of above-mentioned two kinds of solution, put in same silica gel G or GF respectively
254Or on any lamellae among the H, with in n-butyl alcohol-glacial acetic acid-water, n-butyl alcohol-alcohol-water or toluene-ethyl acetate-glacial acetic acid any is developing solvent, the proportioning of three components is 7-25: 1-7: 0.5-2, launch, take out, dry, spray is with 5～50% ethanol solution of sulfuric acid, 100-110 ℃ of baking 5-20 minute.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
Optimized technical scheme of the present invention can be:
The capsular method of quality control that adds lustre to also comprises the following steps:
3. this medicine Chinese crude drug Fructus Lycii is differentiated with thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B):
A. the preparation of control medicinal material solution: get Fructus Lycii control medicinal material 0.5-2g, add water 15-60ml, supersound process 10-40 minute, filter, filtrate is extracted with ethyl acetate 7.5-25ml jolting, and extracting solution is concentrated into 0.5-2ml, makes control medicinal material solution;
B. the preparation of need testing solution: get this product content 0.5-5g, add water 10-100ml, supersound process 10-40 minute, filter, filtrate is extracted with ethyl acetate 5-50ml jolting, and extracting solution is concentrated into 0.5-2ml, makes need testing solution;
C. test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B): draw each 5-20 μ l of above-mentioned two kinds of solution, put in same silica gel G or GF respectively
254Or on any lamellae among the H, with in toluene-ethyl acetate-formic acid, chloroform-ethyl acetate-formic acid or petroleum ether (30～60 ℃)-Ethyl formate-formic acid any is developing solvent, the proportioning of three components is 5-20: 5-20: 0.1-5, launch, take out, dry, put under the uviol lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;
4. this medicine Chinese crude drug Fructus Schisandrae Chinensis is differentiated with thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B):
A. the preparation of control medicinal material solution: get Fructus Schisandrae Chinensis control medicinal material 0.1-1g, add chloroform 6-60ml, reflux 0.1-1 hour, filter, filtrate evaporate to dryness, residue add chloroform 0.5-2ml makes dissolving, makes control medicinal material solution;
B. the preparation of need testing solution: get this product content 1.5-6g, add chloroform 15-60ml, reflux 0.1-1 hour, filter, filtrate evaporate to dryness, residue add chloroform 0.5-2ml makes dissolving, makes need testing solution;
C. test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B): draw need testing solution 3-12 μ l, control medicinal material solution 0.5-2 μ l puts in same silica gel G F respectively
254Or on any lamellae among G or the H, with toluene-ethyl acetate proportioning is that 7-10: 0.5-2 or petroleum ether (30～60 ℃)-Ethyl formate-formic acid proportioning are that in the upper solution of 13-16: 3-6: 0.5-2 any is developing solvent, launch, take out, dry, put under the uviol lamp (254nm) and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
More preferably technical scheme comprises following determination step:
1. measure ferulic acid (C in this medicine with high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 D)
18H
21O
3) content:
A. chromatographic condition: with octadecylsilane chemically bonded silica is filler; Proportioning is 30: 70 a methanol--0.1% phosphoric acid solution is a mobile phase, and the detection wavelength is 320nm;
B. the preparation of reference substance solution: it is an amount of that precision takes by weighing the ferulic acid reference substance, puts in the brown measuring bottle, adds methanol and make the solution that every 1ml contains 15 μ g, promptly;
C. the preparation of need testing solution: get the content of 10 of this product, the accurate title, decided mixing, porphyrize, get 1g, the accurate title, decide, and puts in the tool plug conical flask, the accurate 70% methanol 50ml that adds, claim decide weight, supersound process 1 hour is put coldly, and weight decided in title again, supply the weight that subtracts mistake with 70% methanol, shake up, filter, precision is measured subsequent filtrate 25ml, volatilize, residue adds 70% methanol and is transferred in the 5ml measuring bottle, adds 70% methanol to scale, shake up, filter with 0.45 μ m filter membrane, promptly;
D. content of ferulic acid assay method: accurate respectively each the 10 μ l of reference substance solution and need testing solution that draw, inject chromatograph of liquid, the mensuration content of ferulic acid;
E. every contains Radix Angelicae Sinensis with ferulic acid (C
18H
21O
3) meter, must not be less than 35 μ g;
2. this medicine Chinese crude drug Radix Codonopsis is differentiated with thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B):
A. the preparation of control medicinal material solution: get Radix Codonopsis control medicinal material 2g, add n-butyl alcohol 30ml, reflux 2 hours filters, and filtrate is reclaimed n-butyl alcohol to 2ml, makes control medicinal material solution;
B. the preparation of need testing solution: get this product content 3g, add n-butyl alcohol 30ml, reflux 2 hours filters, and filtrate is reclaimed n-butyl alcohol to 2ml, makes need testing solution;
C. test according to thin layer chromatography: drawing each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, is that n-butyl alcohol-alcohol-water of 25: 3: 2 is developing solvent with proportioning, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, 105 ℃ of bakings 10 minutes.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
The preferred capsular method of quality control that adds lustre to also comprises the following steps: in the above-mentioned more preferably technical scheme steps
3. this medicine Chinese crude drug Fructus Lycii is differentiated with thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B):
A. the preparation of control medicinal material solution: get Fructus Lycii control medicinal material 1g, add water 30ml, supersound process 20 minutes filters, and filtrate is extracted with ethyl acetate 15ml jolting, and extracting solution is concentrated into 1ml, makes control medicinal material solution;
B. the preparation of need testing solution: get this product content 1.5g, add water 30ml, supersound process 20 minutes filters, and filtrate is extracted with ethyl acetate 15ml jolting, and extracting solution is concentrated into 1ml, makes need testing solution;
C. test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B): draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with proportioning is that toluene-ethyl acetate-formic acid of 6: 4: 0.2 is developing solvent, launch, take out, dry, put under the uviol lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;
4. this medicine Chinese crude drug Fructus Schisandrae Chinensis is differentiated with thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B):
A. the preparation of control medicinal material solution: get Fructus Schisandrae Chinensis control medicinal material 0.5g, add chloroform 30ml, reflux 0.5 hour filters, and filtrate evaporate to dryness, residue add chloroform 1ml makes dissolving, makes control medicinal material solution;
B. the preparation of need testing solution: get this product content 3g, add chloroform 30ml, reflux 0.5 hour filters, and filtrate evaporate to dryness, residue add chloroform 1ml makes dissolving, makes need testing solution;
C. test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B): draw need testing solution 6 μ l, control medicinal material solution 1 μ l puts in same silica gel G F respectively
254On the lamellae, be that the upper solution of petroleum ether (30～60 ℃)-Ethyl formate-formic acid of 15: 5: 1 is developing solvent, launch, take out, dry, put under the uviol lamp (254nm) and inspect with proportioning.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
Every the loading amount of capsule of adding lustre to of the present invention is 0.3g.
The TCL that the invention provides Radix Codonopsis, Fructus Lycii and Fructus Schisandrae Chinensis differentiates that having selected the higher ferulic acid of content is the assay index, has set up the capsular HPLC content assaying method that adds lustre to; Through repeated trials repeatedly, confirming should method is simple, the result accurately and reliably, can be used as and add lustre to capsule quality control and investigate the index of technology stability.
The specific embodiment
Embodiment 1: get Chinese crude drug Fructus Lycii 200g, Radix Codonopsis 100g, Radix Angelicae Sinensis 100g, Radix Ophiopogonis 36g, Poria 30g, Rhizoma Alismatis 24g, Cortex Moutan 24g, Fructus Schisandrae Chinensis 18g, Rhizoma Acori Graminei 18g, Radix Polygalae (liquorice beverage system) 18g, above-mentioned raw materials ten flavors, get Fructus Schisandrae Chinensis, Rhizoma Acori Graminei, Poria, Radix Polygalae and Radix Codonopsis 20g, mixed powder is broken into fine powder, sieves; The five tastes such as remaining Radix Codonopsis and remaining Rhizoma Alismatis decoct with water secondary, and collecting decoction filters, and filtrate is condensed into thick paste, adds powder such as Fructus Schisandrae Chinensis, mixing, and drying is pulverized, and incapsulates, and makes 1000, every dress 0.3g; The method of quality control of this medicine comprises the following steps:
(1), measures ferulic acid (C in this medicine with high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 D)
18H
21O
3) content:
A. chromatographic condition: with octadecylsilane chemically bonded silica is filler; Proportioning is that 30: 70 methanol-0.1% phosphoric acid solution is a mobile phase, and the detection wavelength is 320nm;
B. the preparation of reference substance solution: it is an amount of that precision takes by weighing the ferulic acid reference substance, puts in the brown measuring bottle, adds methanol and make the solution that every 1ml contains 15 μ g, promptly;
C. the preparation of need testing solution: get the content of 10 of this product, the accurate title, decided mixing, porphyrize, get 1g, the accurate title, decide, and puts in the tool plug conical flask, the accurate 70% methanol 50ml that adds, claim decide weight, supersound process 1 hour is put coldly, and weight decided in title again, supply the weight that subtracts mistake with 70% methanol, shake up, filter, precision is measured subsequent filtrate 25ml, volatilize, residue adds 70% methanol and is transferred in the 5ml measuring bottle, adds 70% methanol to scale, shake up, filter with 0.45 μ m filter membrane, promptly;
D. content of ferulic acid assay method: accurate respectively each the 10 μ l of reference substance solution and need testing solution that draw, inject chromatograph of liquid, the mensuration content of ferulic acid;
E. every contains Radix Angelicae Sinensis with ferulic acid (C
18H
21O
3) meter, must not be less than 35 μ g;
(2), this medicine Chinese crude drug Radix Codonopsis is differentiated with thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B):
A. the preparation of control medicinal material solution: get Radix Codonopsis control medicinal material 2g, add n-butyl alcohol 30ml, reflux 2 hours filters, and filtrate is reclaimed n-butyl alcohol to 2ml, makes control medicinal material solution;
B. the preparation of need testing solution: get this product content 3g, add n-butyl alcohol 30ml, reflux 2 hours filters, and filtrate is reclaimed n-butyl alcohol to 2ml, makes need testing solution;
C. test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B): draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with proportioning is that n-butyl alcohol-alcohol-water of 25: 3: 2 is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, 105 ℃ of bakings 10 minutes.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
(3), this medicine Chinese crude drug Fructus Lycii is differentiated with thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B):
A. the preparation of control medicinal material solution: get Fructus Lycii control medicinal material 1g, add water 30ml, supersound process 20 minutes filters, and filtrate is extracted with ethyl acetate 15ml jolting, and extracting solution is concentrated into 1ml, makes control medicinal material solution;
B. the preparation of need testing solution: get this product content 1.5g, add water 30ml, supersound process 20 minutes filters, and filtrate is extracted with ethyl acetate 15ml jolting, and extracting solution is concentrated into 1ml, makes need testing solution;
C. test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B): draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with proportioning is that toluene-ethyl acetate-formic acid of 6: 4: 0.2 is developing solvent, launch, take out, dry, put under the uviol lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;
(4), this medicine Chinese crude drug Fructus Schisandrae Chinensis is differentiated with thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B):
A. the preparation of control medicinal material solution: get Fructus Schisandrae Chinensis control medicinal material 0.5g, add chloroform 30ml, reflux 0.5 hour filters, and filtrate evaporate to dryness, residue add chloroform 1ml makes dissolving, makes control medicinal material solution;
B. the preparation of need testing solution: get this product content 3g, add chloroform 30ml, reflux 0.5 hour filters, and filtrate evaporate to dryness, residue add chloroform 1ml makes dissolving, makes need testing solution;
C. test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B): draw need testing solution 6 μ l, control medicinal material solution 1 μ l puts in same silica gel G F respectively
254On the lamellae, be that the upper solution of petroleum ether (30～60 ℃)-Ethyl formate-formic acid of 15: 5: 1 is developing solvent, launch, take out, dry, put under the uviol lamp (254nm) and inspect with proportioning.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
Claims (2)
1. capsular method of quality control that adds lustre to, wherein said pharmaceutical formulation by Chinese crude drug Radix Codonopsis 100g, Radix Angelicae Sinensis 100g, Fructus Lycii 200g, Poria 30g, Radix Ophiopogonis 36g, Rhizoma Alismatis 24g, Fructus Schisandrae Chinensis 18g, Rhizoma Acori Graminei 18g, Cortex Moutan 24g, Radix Polygalae (liquorice beverage system) 18g form, above-mentioned raw materials is made 1000 altogether, it is characterized in that this method comprises the following steps:
(1), with ferulic acid (C in this medicine of high effective liquid chromatography for measuring
18H
21O
3) content:
A. chromatographic condition: with the octadecylsilane chemically bonded silica is filler; Proportioning is that methanol-0.1% phosphoric acid solution of 25-35: 65-75 is a mobile phase, and the detection wavelength is 320 ± 7nm;
B. the preparation of reference substance solution: it is an amount of that precision takes by weighing the ferulic acid reference substance, puts in the brown measuring bottle, adds in methanol or the ethanol any and make the solution that every 1ml contains 5--50 μ g, promptly;
C. the preparation of need testing solution: get the content of this product 2-15 grain, the accurate title, decided mixing, porphyrize is got 0.1-2g, and accurate the title decides, put in the tool plug conical flask, accurate any 10～50ml that adds in 10～100% methanol or the ethanol claims to decide weight, supersound process 0.5-2 hour, put cold, claim to decide weight again, supply the weight that subtracts mistake, shake up with in 10～100% methanol or the ethanol any, filter, precision is measured subsequent filtrate 1-25ml, volatilizes, and residue adds in 10～100% methanol or the ethanol any and is transferred in the 2-10ml measuring bottle, add in 10～100% methanol or the ethanol any to scale, shake up, filter with 0.45 μ m microporous filter membrane, promptly;
D. content of ferulic acid assay method: accurate respectively reference substance solution and each 5--20 μ l of need testing solution of drawing, inject chromatograph of liquid, the mensuration content of ferulic acid;
E. every contains Radix Angelicae Sinensis with ferulic acid (C
18H
21O
3) meter, must not be less than 35 μ g;
(2), this medicine Chinese crude drug Radix Codonopsis is differentiated with thin layer chromatography:
A. the preparation of control medicinal material solution: get Radix Codonopsis control medicinal material 1-5g, add n-butyl alcohol 15-75ml, reflux 1-4 hour, filter, filtrate is reclaimed n-butyl alcohol to 1-5ml, makes control medicinal material solution;
B. the preparation of need testing solution: get this product content 1-5g, add n-butyl alcohol 10-50ml, reflux 1-4 hour, filter, filtrate is reclaimed n-butyl alcohol to 1-5ml, makes need testing solution;
C. test according to thin layer chromatography: draw each 1-15 μ l of above-mentioned two kinds of solution, put in same silica gel G or GF respectively
254Or on any lamellae among the H, with in n-butyl alcohol-glacial acetic acid-water, n-butyl alcohol-alcohol-water or toluene-ethyl acetate-glacial acetic acid any is developing solvent, the proportioning of three components is 7-25: 1-7: 0.5-2, launch, take out, dry, spray is with 5～50% ethanol solution of sulfuric acid, 100～110 ℃ of bakings 5-20 minute.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
(3), this medicine Chinese crude drug Fructus Lycii is differentiated with thin layer chromatography:
A. the preparation of control medicinal material solution: get Fructus Lycii control medicinal material 0.5-2g, add water 15-60ml, supersound process 10-40 minute, filter, filtrate is extracted with ethyl acetate 7.5-25ml jolting, and extracting solution is concentrated into 0.5-2ml, makes control medicinal material solution;
B. the preparation of need testing solution: get this product content 0.5-5g, add water 10-100ml, supersound process 10-40 minute, filter, filtrate is extracted with ethyl acetate 5-50ml jolting, and extracting solution is concentrated into 0.5-2ml, makes need testing solution;
C. test according to thin layer chromatography: draw each 5-20 μ l of above-mentioned two kinds of solution, put in same silica gel G or GF respectively
254Or on any lamellae among the H, with in toluene-ethyl acetate-formic acid, chloroform-ethyl acetate-formic acid or petroleum ether (30～60 ℃)-Ethyl formate-formic acid any is developing solvent, the proportioning of three components is 5-20: 5-20: 0.1-5, launch, take out, dry, put under the uviol lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;
(4), this medicine Chinese crude drug Fructus Schisandrae Chinensis is differentiated with thin layer chromatography: the preparation of a. control medicinal material solution: get Fructus Schisandrae Chinensis control medicinal material 0.1-1g, add chloroform 6-60ml, reflux 0.1-1 hour, filter, the filtrate evaporate to dryness, residue adds chloroform 0.5-2ml makes dissolving, makes control medicinal material solution;
B. the preparation of need testing solution: get this product content 1.5-6g, add chloroform 15-60ml, reflux 0.1-1 hour, filter, filtrate evaporate to dryness, residue add chloroform 0.5-2ml makes dissolving, makes need testing solution;
C. test according to thin layer chromatography: draw need testing solution 3-12 μ l, control medicinal material solution 0.5-2 μ l puts in same silica gel G F respectively
254Or on any lamellae among G or the H, with toluene-ethyl acetate proportioning is that 7-10: 0.5-2 or petroleum ether (30～60 ℃)-Ethyl formate-formic acid proportioning are that in the upper solution of 13-16: 3-6: 0.5-2 any is developing solvent, launch, take out, dry, put under the uviol lamp (254nm) and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
2. the capsular method of quality control that adds lustre to according to claim 1, it is characterized in that this method comprise the following steps: (1), with ferulic acid (C in this medicine of high effective liquid chromatography for measuring
18H
21O
3) content:
A. chromatographic condition: with octadecylsilane chemically bonded silica is filler; Proportioning is that 30: 70 methanol-0.1% phosphoric acid solution is a mobile phase, and the detection wavelength is 320nm;
B. the preparation of reference substance solution: it is an amount of that precision takes by weighing the ferulic acid reference substance, puts in the brown measuring bottle, adds methanol and make the solution that every 1ml contains 15 μ g, promptly;
C. the preparation of need testing solution: get the content of 10 of this product, the accurate title, decided mixing, porphyrize, get 1g, the accurate title, decide, and puts in the tool plug conical flask, the accurate 70% methanol 50ml that adds, claim decide weight, supersound process 1 hour is put coldly, and weight decided in title again, supply the weight that subtracts mistake with 70% methanol, shake up, filter, precision is measured subsequent filtrate 25ml, volatilize, residue adds 70% methanol and is transferred in the 5ml measuring bottle, adds 70% methanol to scale, shake up, filter with 0.45 μ m filter membrane, promptly;
D. content of ferulic acid assay method: accurate respectively each the 10 μ l of reference substance solution and need testing solution that draw, inject chromatograph of liquid, the mensuration content of ferulic acid;
E. every contains Radix Angelicae Sinensis with ferulic acid (C
18H
21O
3) meter, must not be less than 35 μ g;
(2), this medicine Chinese crude drug Radix Codonopsis is differentiated with thin layer chromatography:
A. the preparation of control medicinal material solution: get Radix Codonopsis control medicinal material 2g, add n-butyl alcohol 30ml, reflux 2 hours filters, and filtrate is reclaimed n-butyl alcohol to 2ml, makes control medicinal material solution;
B. the preparation of need testing solution: get this product content 3g, add n-butyl alcohol 30ml, reflux 2 hours filters, and filtrate is reclaimed n-butyl alcohol to 2ml, makes need testing solution;
C. test according to thin layer chromatography: drawing each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, is that n-butyl alcohol-alcohol-water of 25: 3: 2 is developing solvent with proportioning, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, 105 ℃ of bakings 10 minutes.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
(3), this medicine Chinese crude drug Fructus Lycii is differentiated with thin layer chromatography:
A. the preparation of control medicinal material solution: get Fructus Lycii control medicinal material 1g, add water 30ml, supersound process 20 minutes filters, and filtrate is extracted with ethyl acetate 15ml jolting, and extracting solution is concentrated into 1ml, makes control medicinal material solution;
B. the preparation of need testing solution: get this product content 1.5g, add water 30ml, supersound process 20 minutes filters, and filtrate is extracted with ethyl acetate 15ml jolting, and extracting solution is concentrated into 1ml, makes need testing solution;
C. test according to thin layer chromatography: drawing each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, is that toluene-ethyl acetate-formic acid of 6: 4: 0.2 is developing solvent with proportioning, launches, and takes out, and dries, and puts under the uviol lamp (365nm) and inspects.
In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;
(4), this medicine Chinese crude drug Fructus Schisandrae Chinensis is differentiated with thin layer chromatography:
A. the preparation of control medicinal material solution: get Fructus Schisandrae Chinensis control medicinal material 0.5g, add chloroform 30ml, reflux 0.5 hour filters, and filtrate evaporate to dryness, residue add chloroform 1ml makes dissolving, makes control medicinal material solution;
B. the preparation of need testing solution: get this product content 3g, add chloroform 30ml, reflux 0.5 hour filters, and filtrate evaporate to dryness, residue add chloroform 1ml makes dissolving, makes need testing solution;
C. test according to thin layer chromatography: draw need testing solution 6 μ l, control medicinal material solution 1 μ l puts in same silica gel G F respectively
254On the lamellae, be that the upper solution of petroleum ether (30～60 ℃)-Ethyl formate-formic acid of 15: 5: 1 is developing solvent, launch, take out, dry, put under the uviol lamp (254nm) and inspect with proportioning.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103134883A (en) * | 2011-11-28 | 2013-06-05 | 邯郸摩罗丹药业股份有限公司 | Medicine composition and detecting method of manufacturing agent of medicine composition |
| CN103558330A (en) * | 2013-10-08 | 2014-02-05 | 九芝堂股份有限公司 | Thin-layer identification chromatography method of stomach-strengthening ulcer-curing preparation |
| CN107831261A (en) * | 2017-12-13 | 2018-03-23 | 广东心宝药业科技有限公司 | The quality determining method of rhizoma alismatis root bark of tree peony root of herbaceous peony preparation |
| CN111024877A (en) * | 2019-12-30 | 2020-04-17 | 扬州市食品药品检验检测中心 | Method for detecting traditional Chinese medicine components in kidney-tonifying and bone-strengthening pill |
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2010
- 2010-05-07 CN CN2010101650418A patent/CN102233097A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103134883A (en) * | 2011-11-28 | 2013-06-05 | 邯郸摩罗丹药业股份有限公司 | Medicine composition and detecting method of manufacturing agent of medicine composition |
| CN103134883B (en) * | 2011-11-28 | 2015-05-13 | 邯郸制药股份有限公司 | Medicine composition and detecting method of formula of medicine composition |
| CN103558330A (en) * | 2013-10-08 | 2014-02-05 | 九芝堂股份有限公司 | Thin-layer identification chromatography method of stomach-strengthening ulcer-curing preparation |
| CN103558330B (en) * | 2013-10-08 | 2016-01-20 | 九芝堂股份有限公司 | A kind of TLC distinguish chromatographic process of Jianwei Yuyang preparation |
| CN107831261A (en) * | 2017-12-13 | 2018-03-23 | 广东心宝药业科技有限公司 | The quality determining method of rhizoma alismatis root bark of tree peony root of herbaceous peony preparation |
| CN111024877A (en) * | 2019-12-30 | 2020-04-17 | 扬州市食品药品检验检测中心 | Method for detecting traditional Chinese medicine components in kidney-tonifying and bone-strengthening pill |
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Application publication date: 20111109 |