CN101766800B - Quality detection method of pills for treating cold and expelling wind - Google Patents
Quality detection method of pills for treating cold and expelling wind Download PDFInfo
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- CN101766800B CN101766800B CN2010101010962A CN201010101096A CN101766800B CN 101766800 B CN101766800 B CN 101766800B CN 2010101010962 A CN2010101010962 A CN 2010101010962A CN 201010101096 A CN201010101096 A CN 201010101096A CN 101766800 B CN101766800 B CN 101766800B
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- expelling wind
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- treating cold
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- 239000006187 pill Substances 0.000 title claims abstract description 98
- 238000001514 detection method Methods 0.000 title claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 47
- YKRGDOXKVOZESV-WRJNSLSBSA-N Paeoniflorin Chemical compound C([C@]12[C@H]3O[C@]4(O)C[C@](O3)([C@]1(C[C@@H]42)O[C@H]1[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O1)O)C)OC(=O)C1=CC=CC=C1 YKRGDOXKVOZESV-WRJNSLSBSA-N 0.000 claims abstract description 22
- 238000004809 thin layer chromatography Methods 0.000 claims abstract description 18
- 238000002360 preparation method Methods 0.000 claims abstract description 16
- 239000003814 drug Substances 0.000 claims abstract description 13
- BALXUFOVQVENIU-GNAZCLTHSA-N Ephedrine hydrochloride Chemical compound Cl.CN[C@@H](C)[C@H](O)C1=CC=CC=C1 BALXUFOVQVENIU-GNAZCLTHSA-N 0.000 claims abstract description 9
- 229960002534 ephedrine hydrochloride Drugs 0.000 claims abstract description 9
- YKRGDOXKVOZESV-UHFFFAOYSA-N paeoniflorin Natural products O1C(C)(C2(CC34)OC5C(C(O)C(O)C(CO)O5)O)CC3(O)OC1C24COC(=O)C1=CC=CC=C1 YKRGDOXKVOZESV-UHFFFAOYSA-N 0.000 claims abstract description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 60
- 239000013558 reference substance Substances 0.000 claims description 44
- 238000012360 testing method Methods 0.000 claims description 40
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 34
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 16
- 229960004756 ethanol Drugs 0.000 claims description 15
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- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 8
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 8
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- 235000006200 Glycyrrhiza glabra Nutrition 0.000 claims description 4
- PQLVXDKIJBQVDF-UHFFFAOYSA-N acetic acid;hydrate Chemical compound O.CC(O)=O PQLVXDKIJBQVDF-UHFFFAOYSA-N 0.000 claims description 4
- PBCJIPOGFJYBJE-UHFFFAOYSA-N acetonitrile;hydrate Chemical compound O.CC#N PBCJIPOGFJYBJE-UHFFFAOYSA-N 0.000 claims description 4
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 4
- 229920003123 carboxymethyl cellulose sodium Polymers 0.000 claims description 4
- 229940063834 carboxymethylcellulose sodium Drugs 0.000 claims description 4
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- 229960000935 dehydrated alcohol Drugs 0.000 claims description 4
- 239000000428 dust Substances 0.000 claims description 4
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 4
- 239000000835 fiber Substances 0.000 claims description 4
- 239000000945 filler Substances 0.000 claims description 4
- 239000000706 filtrate Substances 0.000 claims description 4
- LPLVUJXQOOQHMX-QWBHMCJMSA-N glycyrrhizinic acid Chemical compound O([C@@H]1[C@@H](O)[C@H](O)[C@H](O[C@@H]1O[C@@H]1C([C@H]2[C@]([C@@H]3[C@@]([C@@]4(CC[C@@]5(C)CC[C@@](C)(C[C@H]5C4=CC3=O)C(O)=O)C)(C)CC2)(C)CC1)(C)C)C(O)=O)[C@@H]1O[C@H](C(O)=O)[C@@H](O)[C@H](O)[C@H]1O LPLVUJXQOOQHMX-QWBHMCJMSA-N 0.000 claims description 4
- 239000004816 latex Substances 0.000 claims description 4
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- 235000011477 liquorice Nutrition 0.000 claims description 4
- FEMOMIGRRWSMCU-UHFFFAOYSA-N ninhydrin Chemical compound C1=CC=C2C(=O)C(O)(O)C(=O)C2=C1 FEMOMIGRRWSMCU-UHFFFAOYSA-N 0.000 claims description 4
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 claims description 4
- 238000010992 reflux Methods 0.000 claims description 4
- 229920006395 saturated elastomer Polymers 0.000 claims description 4
- 230000028327 secretion Effects 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 4
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 239000006228 supernatant Substances 0.000 claims description 4
- 238000011003 system suitability test Methods 0.000 claims description 4
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- 239000002253 acid Substances 0.000 claims description 3
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- 239000001117 sulphuric acid Substances 0.000 claims description 3
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- 238000004811 liquid chromatography Methods 0.000 claims description 2
- 229940079593 drug Drugs 0.000 abstract description 9
- 238000003908 quality control method Methods 0.000 abstract description 6
- 230000005180 public health Effects 0.000 abstract description 5
- 241000202807 Glycyrrhiza Species 0.000 abstract description 3
- 150000001875 compounds Chemical class 0.000 abstract description 3
- LTINPJMVDKPJJI-UHFFFAOYSA-N iodinated glycerol Chemical compound CC(I)C1OCC(CO)O1 LTINPJMVDKPJJI-UHFFFAOYSA-N 0.000 abstract description 3
- 241001465251 Ephedra sinica Species 0.000 abstract description 2
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- 208000026435 phlegm Diseases 0.000 description 3
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- Medicines Containing Plant Substances (AREA)
Abstract
The invention relates to a quality detection method of pills for treating cold and expelling cold in volume 13 of Drug Standard of Ministry of Public Health of the Peoples Republic of China (traditional Chinese medicine set prescription preparation). The quality detection method of the pills for treating cold and expelling wind improves the quality control standard of the pills for treating cold and expelling wind, establishes measurement indexes of contents in a preparation and a detection method thereof, adds a thin-layer chromatography qualitative identification method of ephedrine hydrochloride and glycyrrhiza which are main constituents in Chinese ephedra as a main drug, improves a thin-layer chromatography identification method of paeoniflorin and ensures that the method is simpler, and the compound preparation has higher quality standard level.
Description
Technical field
The present invention relates to the quality determining method of pills for treating cold and expelling wind in the 13 in " Drug Standard of Ministry of Public Health of the Peoples Republic of China " (Chinese traditional patent formulation preparation).
Background technology
Medicine pills for treating cold and expelling wind in the 13 in " Drug Standard of Ministry of Public Health of the Peoples Republic of China " (Chinese traditional patent formulation preparation) has relieving the exterior syndrome with drugs of pungent in flavor and warm in nature, lung qi dispersing with in effect; Be used for anemofrigid cold, fever and cough, headache is afraid of cold; Rhinorrhea with clear discharge, joint is ached, and extremity are tired.This compound preparation by Chinese crude drug Herba Ephedrae (processing) 50g, Semen Armeniacae Amarum 75g, Ramulus Cinnamomi 75g, the Radix Paeoniae Alba (wine is processed) 125g, Folium Perillae 50g, windproof 75g, Radix Angelicae Pubescentis 50g, Radix Platycodonis 50g,, Fructus Setariae Germinatus (stir-fry) 125g, Radix Glycyrrhizae 50g, Fructus Jujubae (enucleation) 75g, Rhizoma Zingiberis Recens (smashing to pieces) 50g form.Herba Ephedrae is the dry herb stem of Ephedraceae plant plait Herba Ephedrae Ephedra sinica Stapf, epheday intermedia Ephedra intermedia Schrenk et C.A.Mey. or ephedra equisetina Ephedra equisetina Bge.; Tool diaphoresis cold expelling, the effect of depressed lung-energy dispersing; Semen Armeniacae Amarum is the dry mature seed of rosaceous plant Prunus armeniaca L.var.ansu Maxim. Prunus armeniaca L.var.ansu Maxim., Siberia Fructus Pruni Prunus sibirica L., prunus mandshuricaKoehne Prunus mandshurica (Maxim.) Koehne or Fructus Pruni Prunus armeniaca L., has the effect of sending down the abnormal ascending QI relieving cough and asthma; Ramulus Cinnamomi is the dry twig of canella Cortex Cinnamomi Cinnamomum cassia Presl, has the effect of diaphoresis expelling pathogenic factors from muscles; The Radix Paeoniae Alba is the dry root of ranunculaceae plant Radix Paeoniae Paeonia lactiflora Pall., has the suppressing the hyperactive liver pain relieving, the effect of astringing YIN to stop sweating; Folium Perillae is the dried leaves (or band twig) of labiate Folium Perillae Perilla frutescens (L.) Britt, has the effect of the cold expelling of inducing sweat; Windproof is the dry root of umbelliferae Saposhnikovia divaricata Saposhnikovia divaricata (Turcz.) Schischk., the effect of tool inducing diaphoresis to dispel wind; Radix Angelicae Pubescentis is the dry root of the heavy peristome Radix Angelicae Sinensis of samphire Angelica pubescens Maxim.f.biserrata Shan et Yuan, tool expelling wind and removing dampness, the effect of numbness relieving and pain relieving; Radix Platycodonis is the dry root of campanulaceae Platycodon grandiflouorum Platycodon grandiflorum (Jacq.) A.DC., has lung qi dispersing, and sore-throat relieving eliminates the phlegm, the effect of evacuation of pus; Fructus Setariae Germinatus is that the mature fruit of grass foxtail millet Setaria italica (L.) Beauv. gets through the drying of germinateing, tool help digestion with in effect; Radix Glycyrrhizae is the dry root and rhizome of glycyrrhizic legume Glycyrrhiza inflataBat., Glycyrrhiza inflata Bat. Glycyrrhiza in flata Bat or Glycyrrhiza glabra L. Glycyrrhiza glabra L.; Have invigorating the spleen and replenishing QI, heat-clearing and toxic substances removing, expelling phlegm for arresting cough, the effect of coordinating the actions of various ingredients in a prescription; Fructus Jujubae is the dry mature fruit of Rhamnaceae plant Fructus Jujubae Ziziphus jujubaMill., the effect of tool invigorating the spleen and replenishing QI; These article are the fresh rhizome of zingiber Zingiber officinale Rosc., the tool cold expelling that induces sweat, warming middle-JIAO to arrest vomiting, the effect of preventing phlegm from forming and stopping coughing." Drug Standard of Ministry of Public Health of the Peoples Republic of China " the 13 quality control standard (WS that has issued pills for treating cold and expelling wind
3-B-2632-97), but in the existing pills for treating cold and expelling wind method of quality control that Ministry of Public Health is issued, have only microscopical identification and thin layer to differentiate that limitation is very big, is difficult to accurately control the quality of pills for treating cold and expelling wind.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, a kind of quality determining method of pills for treating cold and expelling wind is provided, to improve the quality control standard of pills for treating cold and expelling wind.
The medicine of pills for treating cold and expelling wind is by Herba Ephedrae (processing) 50g; Semen Armeniacae Amarum 75g; Ramulus Cinnamomi 75g; The Radix Paeoniae Alba (wine is processed) 125g; Folium Perillae 50g; Windproof 75g; Radix Angelicae Pubescentis 50g; Radix Platycodonis 50g; Fructus Setariae Germinatus (stir-fry) 125g; Radix Glycyrrhizae 50g; Fructus Jujubae (enucleation) 75g; Rhizoma Zingiberis Recens (smashing to pieces) 50g forms, and processes water-honeyed pill or big honeyed pills.
The quality determining method of pills for treating cold and expelling wind of the present invention is following:
1, differentiates
1) get pills for treating cold and expelling wind, put microscopically and observe: calcium oxalate cluster crystal diameter 18～32 μ m, be present in the parenchyma cell, often arrange in a row, or contain several cluster crystals in a cell.The stone cell class is square, and wall is simultaneously poor.Oil pipe contains golden yellow secretions, diameter 17～60 μ m.Connect latex dust diameter 14～25 μ m, contain faint yellow granular substance.Parenchyma cell contains prism of calcium oxalate around the fibre bundle, forms crystalline cellulose.Stone cell is orange-yellow, shell-like, and wall is thicker, and pit is obvious on one side for broad;
2) the thin layer chromatography discrimination method of ephedrine hydrochloride: get pills for treating cold and expelling wind water-honeyed pill 10g, porphyrize; Or get big honeyed pills 1 ball, and shred, add kieselguhr 2-4g, grind well; Add water 2-3ml and make moisteningly, add strong ammonia solution 2-3ml and chloroform 30-40ml reflux 20-60 minute again, filter; Filtrating is steamed near and is done, and residue adds methanol 0.5-1ml makes dissolving, as need testing solution; Other gets the ephedrine hydrochloride reference substance, adds methanol and processes the solution that every 1ml contains 1mg, as reference substance solution; According to thin layer chromatography test, draw need testing solution 8～15 μ l, reference substance solution 5 μ l, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose; By volume proportioning 18-22: 3-4: 0.4-0.6 is as developing solvent with chloroform-methanol-strong ammonia solution, and expansion is taken out; Dry, spray is with ninhydrin solution, and it is clear to be heated to speckle colour developing at 100-110 ℃; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
3) the thin layer chromatography discrimination method of the peoniflorin in the Radix Glycyrrhizae and the Radix Paeoniae Alba: get pills for treating cold and expelling wind water-honeyed pill 12g, porphyrize; Or get big honeyed pills 1 ball, and shred, add kieselguhr 3-4g, grind well; Add water saturated n-butyl alcohol 30-40ml, supersound process 20-60 minute, put coldly, filter; Filtrating is with the saturated water washing of n-butyl alcohol 1-3 time, and 20-30ml obtains n-butyl alcohol liquid at every turn; Evaporate to dryness, residue add dehydrated alcohol 1-2ml makes dissolving, as need testing solution; In addition extracting liquorice control medicinal material 0.5g adds water saturated n-butyl alcohol 5-15ml, and supersound process 20-60 minute, put coldly, filter, the filtrating evaporate to dryness, residue adds methanol 1ml makes dissolving, as Radix Glycyrrhizae control medicinal material solution; Other gets the peoniflorin reference substance and adds methanol and process the solution that every 1ml contains 1mg, as reference substance solution; According to thin layer chromatography test, draw each 5 μ l of need testing solution 10～20 μ l and above-mentioned control medicinal material solution and reference substance solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the carboxymethylcellulose sodium solution that contains 1% (g/ml) sodium hydroxide; With ethyl acetate-formic acid-glacial acetic acid-water proportioning 14-16: 0.9-1.1: 0.9-1.1 by volume: 1.8-2.2 is as developing solvent; Launch, open up, take out to more than the 12cm; Dry; Spray is that 1.0ml sulphuric acid adds the solution that ethanol makes into 10ml with ethanol solution of sulfuric acid (1 → 10), and it is clear to be heated to speckle colour developing at 100-110 ℃, in the test sample chromatograph; With reference substance chromatograph and the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
2, content of paeoniflorin assay method in the pills for treating cold and expelling wind: according to high effective liquid chromatography for measuring
(1) chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filler; With acetonitrile-water by volume proportioning 13: 87 as mobile phase; The detection wavelength is 230 ± 2nm;
(2) preparation of reference substance solution: it is an amount of that precision takes by weighing the peoniflorin reference substance, adds methanol and process the solution that every 1ml contains 80-90 μ g, promptly gets;
(3) preparation of need testing solution: get the pills for treating cold and expelling wind water-honeyed pill, porphyrize is got about 1-2g, and accurate the title decides; Or get the pills for treating cold and expelling wind big honeyed pills, and shredding, mixing is got about 1.5g, and accurate the title, decide; Put in the tool plug conical flask, the accurate 50% ethanol 25-50ml that adds, close plug is claimed to decide weight, supersound process 30-50 minute; The big honeyed pills supersound process is to dissolve loosing it, puts coldly, claims to decide weight again, supplies the weight that subtracts mistake with 50% ethanol, shakes up; Centrifugal 2～5 minutes, get supernatant, filter, get subsequent filtrate, promptly get;
(4) algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly get, pills for treating cold and expelling wind contains the Radix Paeoniae Alba in peoniflorin, and the every 1g of water-honeyed pill must not be less than 1.4mg; The every ball of big honeyed pills must not be less than 6.0mg;
Wherein, contain the some grams of solute among the every 100ml of " % (g/ml) " expression solution; Alcoholic acid percentage ratio means the ratio of capacity in the time of 20 ℃.
The quality determining method of pills for treating cold and expelling wind of the present invention; Improve the quality control standard of pills for treating cold and expelling wind, set up assay index and detection method thereof in the preparation, increased wherein main component ephedrine hydrochloride in the principal agent Herba Ephedrae; The thin layer chromatography qualitative identification method of Radix Glycyrrhizae; Improve the thin layer chromatography discrimination method of peoniflorin, made its method simpler, guaranteed this compound preparation higher quality standard level.
The specific embodiment
Embodiment:
The medicine of pills for treating cold and expelling wind is by Herba Ephedrae (processing) 50g; Semen Armeniacae Amarum 75g; Ramulus Cinnamomi 75g; The Radix Paeoniae Alba (wine is processed) 125g; Folium Perillae 50g; Windproof 75g; Radix Angelicae Pubescentis 50g; Radix Platycodonis 50g; Fructus Setariae Germinatus (stir-fry) 125g; Radix Glycyrrhizae 50g; Fructus Jujubae (enucleation) 75g; Rhizoma Zingiberis Recens (smashing to pieces) 50g forms.
Method for making: above 12 flavors, be ground into fine powder, sieve mixing; Every 100g powder adds refined honey 40～50g and an amount of water, general ball, and drying, the active carbon coating is processed water-honeyed pill; Or add refined honey 120～140g, and process big honeyed pills, promptly get.
Character: these article be black water-honeyed pill, ball heart yellowish-brown to sepia, or yellowish-brown to pitchy big honeyed pills; It is sweet, bitter, slightly numb puckery to distinguish the flavor of.
The quality determining method of pills for treating cold and expelling wind of the present invention is following:
1, differentiates
1) get pills for treating cold and expelling wind, put microscopically and observe: calcium oxalate cluster crystal diameter 18～32 μ m, be present in the parenchyma cell, often arrange in a row, or contain several cluster crystals in a cell.The stone cell class is square, and wall is simultaneously poor.Oil pipe contains golden yellow secretions, diameter 17～60 μ m.Connect latex dust diameter 14～25 μ m, contain faint yellow granular substance.Parenchyma cell contains prism of calcium oxalate around the fibre bundle, forms crystalline cellulose.Stone cell is orange-yellow, shell-like, and wall is thicker, and pit is obvious on one side for broad;
2) the thin layer chromatography discrimination method of ephedrine hydrochloride: get pills for treating cold and expelling wind water-honeyed pill 10g, porphyrize; Or get big honeyed pills 1 ball, and shred, add kieselguhr 3g, grind well, add water 2ml and make moisteningly, add strong ammonia solution 2ml and chloroform 30ml reflux 30 minutes again, filter, filtrating is steamed near and is done, and residue adds methanol 1ml makes dissolving, as need testing solution; Other gets the ephedrine hydrochloride reference substance, adds methanol and processes the solution that every 1ml contains 1mg, as reference substance solution; According to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B) test, draw need testing solution 8～15 μ l, reference substance solution 5 μ l, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose; With chloroform-methanol-strong ammonia solution (volume proportion 20: 3.5: 0.5) is developing solvent, launches, and takes out; Dry; Spray is with ninhydrin solution, and it is clear to be heated to the speckle colour developing at 105 ℃, in the test sample chromatograph; With the corresponding position of reference substance chromatograph on, show the speckle of same color;
3) the thin layer chromatography discrimination method of the peoniflorin in the Radix Glycyrrhizae and the Radix Paeoniae Alba: get pills for treating cold and expelling wind water-honeyed pill 12g, porphyrize; Or get big honeyed pills 1 ball, and shred, add kieselguhr 3g, grind well, add water saturated n-butyl alcohol 30ml; Supersound process 30 minutes is put coldly, filters, and filtrating is with the saturated water washing of n-butyl alcohol 2 times, 20ml at every turn; Obtain n-butyl alcohol liquid, evaporate to dryness, residue add dehydrated alcohol 1ml makes dissolving, as need testing solution; In addition extracting liquorice control medicinal material 0.5g adds water saturated n-butyl alcohol 10ml, and supersound process 30 minutes is put coldly, filter, and the filtrating evaporate to dryness, residue adds methanol 1ml makes dissolving, as Radix Glycyrrhizae control medicinal material solution; Other gets the peoniflorin reference substance and adds methanol and process the solution that every 1ml contains 1mg, as reference substance solution; According to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B) test, draw each 5 μ l of need testing solution 10～15 μ l and above-mentioned control medicinal material solution and reference substance solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the carboxymethylcellulose sodium solution that contains 1% (g/ml) sodium hydroxide; With ethyl acetate-formic acid-glacial acetic acid-water (volume proportion 15: 1: 1: 2) be developing solvent; Launch, open up, take out to more than the 12cm; Dry; Spray is with ethanol solution of sulfuric acid (1 → 10) (meaning that 1.0ml sulphuric acid adds the solution that ethanol makes into 10ml), and it is clear to be heated to the speckle colour developing at 105 ℃, in the test sample chromatograph; With reference substance chromatograph and the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
2, content of paeoniflorin assay method in the pills for treating cold and expelling wind: measure according to HPLC (an appendix VI of Chinese Pharmacopoeia version in 2005 D):
1) chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filler; With acetonitrile-water (volume proportion 13: 87) is mobile phase; The detection wavelength is 230nm, and number of theoretical plate calculates by the peoniflorin peak should be not less than 2000;
2) preparation of reference substance solution: it is an amount of that precision takes by weighing the peoniflorin reference substance, adds methanol and process the solution that every 1ml contains 85 μ g, promptly gets;
3) preparation of need testing solution: get the pills for treating cold and expelling wind water-honeyed pill, porphyrize is got about 1g, and accurate the title decides; Or get the pills for treating cold and expelling wind big honeyed pills, and shredding, mixing is got about 1.5g, and accurate the title, decide; Put in the tool plug conical flask, the accurate 50% ethanol 25ml that adds, close plug claims to decide weight, supersound process (power 160w; Frequency 50kHz) 30 minutes (the big honeyed pills supersound process is to it dissolve to be loose) put coldly, claims to decide weight again, supplies the weight that subtracts mistake with 50% ethanol, shakes up; It is centrifugal that (rotating speed 4000 γ/min) 2 minutes get supernatant, filter, and get subsequent filtrate, promptly get;
4) algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly get, pills for treating cold and expelling wind contains the Radix Paeoniae Alba with peoniflorin (C
23H
28O
11) meter, the every 1g of water-honeyed pill must not be less than 1.4mg; The every ball of big honeyed pills must not be less than 6.0mg.
Wherein, contain the some grams of solute among the every 100ml of " % (g/ml) " expression solution; Alcoholic acid percentage ratio means the ratio of capacity in the time of 20 ℃.
The quality control standard of the pills for treating cold and expelling wind after the improvement is following:
The pills for treating cold and expelling wind quality standard
Pills for treating cold and expelling wind
Ganmao?Shufeng?Wan
[prescription] Herba Ephedrae (processing) 50g Semen Armeniacae Amarum 75g Ramulus Cinnamomi 75g
The windproof 75g of the Radix Paeoniae Alba (wine is processed) 125g Folium Perillae 50g
Radix Angelicae Pubescentis 50g Radix Platycodonis 50g Fructus Setariae Germinatus (stir-fry) 125g
Radix Glycyrrhizae 50g Fructus Jujubae (enucleation) 75g Rhizoma Zingiberis Recens (smashing to pieces) 50g
[method for making] above 12 flavors are ground into fine powder, sieve mixing.Every 100g powder adds refined honey 40～50g and an amount of water, general ball, and drying, the active carbon coating is processed water-honeyed pill; Or add refined honey 120～140g, and process big honeyed pills, promptly get.
[character] these article be black water-honeyed pill, ball heart yellowish-brown to sepia, or yellowish-brown to pitchy big honeyed pills; It is sweet, bitter, slightly numb puckery to distinguish the flavor of.
These article are got in [discriminating] (1), put microscopically and observe: calcium oxalate cluster crystal diameter 18～32 μ m, be present in the parenchyma cell, and often arrange in a row, or contain several cluster crystals in a cell.The stone cell class is square, and wall is simultaneously poor.Oil pipe contains golden yellow secretions, diameter 17～60 μ m.Connect latex dust diameter 14～25 μ m, contain faint yellow granular substance.Parenchyma cell contains prism of calcium oxalate around the fibre bundle, forms crystalline cellulose.Stone cell is orange-yellow, shell-like, and wall is thicker, and pit is obvious on one side for broad.
(2) get these article water-honeyed pill 10g, porphyrize; Or get big honeyed pills 1 ball, and shred, add kieselguhr 3g, grind well, add water 2ml and make moisteningly, add strong ammonia solution 2ml and chloroform 30ml reflux 30 minutes again, filter, filtrating is steamed near and is done, and residue adds methanol 1ml makes dissolving, as need testing solution.Other gets the ephedrine hydrochloride reference substance, adds methanol and processes the solution that every 1ml contains 1mg, as reference substance solution.According to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005) test, draw need testing solution 8～15 μ l, reference substance solution 5 μ l, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose; With chloroform-methanol-strong ammonia solution (20: 3.5: 0.5) is developing solvent; Launch, take out, dry; Spray is with ninhydrin solution, and it is clear to be heated to the speckle colour developing at 105 ℃.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
(3) get these article water-honeyed pill 12g, porphyrize; Or get big honeyed pills 1 ball, and shred, add kieselguhr 3g, grind well, add water saturated n-butyl alcohol 30ml; Supersound process 30 minutes is put coldly, filters, and filtrating is with the saturated water washing of n-butyl alcohol 2 times, 20ml at every turn; Obtain n-butyl alcohol liquid, evaporate to dryness, residue add dehydrated alcohol 1ml makes dissolving, as need testing solution.In addition extracting liquorice control medicinal material 0.5g adds water saturated n-butyl alcohol 10ml, and supersound process 30 minutes is put coldly, filter, and the filtrating evaporate to dryness, residue adds methanol 1ml makes dissolving, as Radix Glycyrrhizae control medicinal material solution.Other gets the peoniflorin reference substance and adds methanol and process the solution that every 1ml contains 1mg, as reference substance solution.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005); Draw each 5 μ l of need testing solution 10～15 μ l and above-mentioned control medicinal material solution and reference substance solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the carboxymethylcellulose sodium solution that contains 1% sodium hydroxide, with ethyl acetate-formic acid-glacial acetic acid-water (15: 1: 1: 2) be developing solvent; Launch; Open up to more than the 12cm, take out, dry; Spray is with ethanol solution of sulfuric acid (1 → 10), and it is clear to be heated to the speckle colour developing at 105 ℃.In the test sample chromatograph, with reference substance chromatograph and the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
[inspection] should meet each item regulation (an appendix I of Chinese Pharmacopoeia version in 2005 A) relevant under the pill item.
[assay] measured according to HPLC (an appendix VI of Chinese Pharmacopoeia version in 2005 D).
Chromatographic condition and system suitability test are filler with the octadecylsilane chemically bonded silica; With acetonitrile-water (13: 87) is mobile phase; The detection wavelength is 230nm.Number of theoretical plate calculates by the peoniflorin peak should be not less than 2000.
It is an amount of that the preparation precision of reference substance solution takes by weighing the peoniflorin reference substance, adds methanol and process the solution that every 1ml contains 85 μ g, promptly gets.
These article water-honeyed pill is got in the preparation of need testing solution, and porphyrize is got about 1g, and accurate the title decides; Or get the big honeyed pills under the weight differential item, and shredding, mixing is got about 1.5g, and accurate the title, decide; Put in the tool plug conical flask, the accurate 50% ethanol 25ml that adds, close plug claims to decide weight, supersound process (power 160w; Frequency 50kHz) 30 minutes (the big honeyed pills supersound process is to it dissolve to be loose) put coldly, claims to decide weight again, supplies the weight that subtracts mistake with 50% ethanol, shakes up; It is centrifugal that (rotating speed 4000 γ/min) 2 minutes get supernatant, filter, and get subsequent filtrate, promptly get.
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, and promptly get.
These article contain the Radix Paeoniae Alba with peoniflorin (C
23H
28O
11) meter, the every 1g of water-honeyed pill must not be less than 1.4mg; The every ball of big honeyed pills must not be less than 6.0mg.
[function cures mainly] relieving the exterior syndrome with drugs of pungent in flavor and warm in nature, lung qi dispersing with in.Be used for anemofrigid cold, fever and cough, headache is afraid of cold, rhinorrhea with clear discharge, joint is ached, and extremity are tired.
[usage and dosage] is oral, 6g of water-honeyed pill, one time 1 ball of big honeyed pills, 2 times on the one.
The heavy 9g of the every ball of [specification] big honeyed pills; Every bag of 6g of water-honeyed pill.
[storage] sealing.
Claims (1)
1. the detection method of a pills for treating cold and expelling wind, the medicine of pills for treating cold and expelling wind is by Herba Ephedrae (processed) 50g; Semen Armeniacae Amarum 75g; Ramulus Cinnamomi 75g; Radix Paeoniae Alba (processed with wine) 125g; Folium Perillae 50g; Windproof 75g; Radix Angelicae Pubescentis 50g; Radix Platycodonis 50g; Fructus Setariae Germinatus (parched) 125g; Radix Glycyrrhizae 50g; Fructus Jujubae (pitted) 75g; Smash Rhizoma Zingiberis Recens 50g to pieces and form, and process water-honeyed pill or big honeyed pills; The quality determining method that it is characterized in that pills for treating cold and expelling wind is following:
1) get pills for treating cold and expelling wind, put microscopically and observe: calcium oxalate cluster crystal diameter 18～32 μ m, be present in the parenchyma cell, often arrange in a row, or contain several cluster crystals in a cell; The stone cell class is square, and wall is simultaneously poor, and oil pipe contains golden yellow secretions, diameter 17～60 μ m; Connect latex dust diameter 14～25 μ m, contain faint yellow granular substance, parenchyma cell contains prism of calcium oxalate around the fibre bundle, forms crystalline cellulose; Stone cell is orange-yellow, shell-like, and wall is thicker, and pit is obvious on one side for broad;
2) the thin layer chromatography discrimination method of ephedrine hydrochloride: get pills for treating cold and expelling wind water-honeyed pill 10g, porphyrize; Or get big honeyed pills 1 ball, and shred, add kieselguhr 2-4g, grind well; Add water 2-3ml and make moisteningly, add strong ammonia solution 2-3ml and chloroform 30-40ml reflux 20-60 minute again, filter; Filtrating is steamed near and is done, and residue adds methanol 0.5-1ml makes dissolving, as need testing solution; Other gets the ephedrine hydrochloride reference substance, adds methanol and processes the solution that every 1ml contains 1mg, as reference substance solution; According to thin layer chromatography test, draw need testing solution 8～15 μ l, reference substance solution 5 μ l, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose; By volume proportioning 18-22: 3-4: 0.4-0.6 is as developing solvent with chloroform-methanol-strong ammonia solution, and expansion is taken out; Dry, spray is with ninhydrin solution, and it is clear to be heated to speckle colour developing at 100-110 ℃; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
3) the thin layer chromatography discrimination method of the peoniflorin in the Radix Glycyrrhizae and the Radix Paeoniae Alba: get pills for treating cold and expelling wind water-honeyed pill 12g, porphyrize; Or get big honeyed pills 1 ball, and shred, add kieselguhr 3-4g, grind well; Add water saturated n-butyl alcohol 30-40ml, supersound process 20-60 minute, put coldly, filter; Filtrating is with the saturated water washing of n-butyl alcohol 1-3 time, and 20-30ml obtains n-butyl alcohol liquid at every turn; Evaporate to dryness, residue add dehydrated alcohol 1-2ml makes dissolving, as need testing solution; In addition extracting liquorice control medicinal material 0.5g adds water saturated n-butyl alcohol 5-15ml, and supersound process 20-60 minute, put coldly, filter, the filtrating evaporate to dryness, residue adds methanol 1ml makes dissolving, as Radix Glycyrrhizae control medicinal material solution; Other gets the peoniflorin reference substance and adds methanol and process the solution that every 1ml contains 1mg, as reference substance solution; According to thin layer chromatography test, draw each 5 μ l of need testing solution 10～20 μ l and above-mentioned control medicinal material solution and reference substance solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the carboxymethylcellulose sodium solution that contains 1% (g/ml) sodium hydroxide; With ethyl acetate-formic acid-glacial acetic acid-water proportioning 14-16: 0.9-1.1: 0.9-1.1 by volume: 1.8-2.2 is as developing solvent; Launch, open up, take out to more than the 12cm; Dry; Spray is that 1.0ml sulphuric acid adds the solution that ethanol makes into 10ml with ethanol solution of sulfuric acid (1 → 10), and it is clear to be heated to speckle colour developing at 100-110 ℃, in the test sample chromatograph; With reference substance chromatograph and the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
4) content of paeoniflorin assay method in the pills for treating cold and expelling wind: according to high effective liquid chromatography for measuring
(1) chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filler; With acetonitrile-water by volume proportioning 13: 87 as mobile phase; The detection wavelength is 230 ± 2nm;
(2) preparation of reference substance solution: it is an amount of that precision takes by weighing the peoniflorin reference substance, adds methanol and process the solution that every 1ml contains 80-90 μ g, promptly gets;
(3) preparation of need testing solution: get the pills for treating cold and expelling wind water-honeyed pill, porphyrize is got about 1-2g, and accurate the title decides; Or get the pills for treating cold and expelling wind big honeyed pills, and shredding, mixing is got about 1.5g, and accurate the title, decide; Put in the tool plug conical flask, the accurate 50% ethanol 25-50ml that adds, close plug is claimed to decide weight, supersound process 30-50 minute; The big honeyed pills supersound process is to dissolve loosing it, puts coldly, claims to decide weight again, supplies the weight that subtracts mistake with 50% ethanol, shakes up; Centrifugal 2～5 minutes, get supernatant, filter, get subsequent filtrate, promptly get;
(4) algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly get, pills for treating cold and expelling wind contains the Radix Paeoniae Alba in peoniflorin, and the every 1g of water-honeyed pill must not be less than 1.4mg; The every ball of big honeyed pills must not be less than 6.0mg;
Wherein, contain the some grams of solute among the every 100ml of " % (g/ml) " expression solution; Alcoholic acid percentage ratio means the ratio of capacity in the time of 20 ℃.
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