CN102507781B - Method for controlling quality of medicine for treating rheumatism and apoplexy diseases - Google Patents
Method for controlling quality of medicine for treating rheumatism and apoplexy diseases Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 50
- 239000003814 drug Substances 0.000 title claims abstract description 38
- 206010008190 Cerebrovascular accident Diseases 0.000 title claims abstract description 15
- 208000006011 Stroke Diseases 0.000 title claims abstract description 15
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 claims abstract description 36
- 238000001514 detection method Methods 0.000 claims abstract description 21
- 238000004809 thin layer chromatography Methods 0.000 claims abstract 5
- 239000000243 solution Substances 0.000 claims description 90
- 238000012360 testing method Methods 0.000 claims description 50
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- 235000018167 Reynoutria japonica Nutrition 0.000 claims description 23
- 240000001341 Reynoutria japonica Species 0.000 claims description 23
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- -1 2,3,5,4 '-tetrahydroxystilbene-2-O-β-D-Glucose glycosides Chemical class 0.000 claims description 16
- 239000003292 glue Substances 0.000 claims description 15
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- 240000007551 Boswellia serrata Species 0.000 claims description 14
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- 239000004863 Frankincense Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
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- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 10
- 229930182470 glycoside Natural products 0.000 claims description 10
- 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 9
- 239000007767 bonding agent Substances 0.000 claims description 9
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- 239000000741 silica gel Substances 0.000 claims description 9
- 229910002027 silica gel Inorganic materials 0.000 claims description 9
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 9
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 8
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 229930013930 alkaloid Natural products 0.000 claims description 8
- 239000000945 filler Substances 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 claims description 8
- 239000002775 capsule Substances 0.000 claims description 7
- 238000004811 liquid chromatography Methods 0.000 claims description 7
- 239000006187 pill Substances 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 7
- 238000003556 assay Methods 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 239000007921 spray Substances 0.000 claims description 5
- 239000012085 test solution Substances 0.000 claims description 5
- FRPHFZCDPYBUAU-UHFFFAOYSA-N Bromocresolgreen Chemical compound CC1=C(Br)C(O)=C(Br)C=C1C1(C=2C(=C(Br)C(O)=C(Br)C=2)C)C2=CC=CC=C2S(=O)(=O)O1 FRPHFZCDPYBUAU-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
- 229910021529 ammonia Inorganic materials 0.000 claims description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N formic acid Substances OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 4
- 239000000395 magnesium oxide Substances 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 238000004448 titration Methods 0.000 claims description 4
- MWOOGOJBHIARFG-UHFFFAOYSA-N vanillin Chemical compound COC1=CC(C=O)=CC=C1O MWOOGOJBHIARFG-UHFFFAOYSA-N 0.000 claims description 4
- 241000282894 Sus scrofa domesticus Species 0.000 claims description 3
- 241000173529 Aconitum napellus Species 0.000 claims description 2
- 239000011435 rock Substances 0.000 claims description 2
- 238000003908 quality control method Methods 0.000 abstract description 16
- 238000000691 measurement method Methods 0.000 abstract 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 84
- 239000013558 reference substance Substances 0.000 description 31
- 239000000047 product Substances 0.000 description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 23
- 238000004587 chromatography analysis Methods 0.000 description 16
- 239000000706 filtrate Substances 0.000 description 12
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 6
- 238000002347 injection Methods 0.000 description 6
- 239000007924 injection Substances 0.000 description 6
- DPMGVDIWDTYPMP-UHFFFAOYSA-N Hypaconitine Natural products COCC12CCC(OC)C3(CN(C)C1)C4CC5(O)C(OC)C(O)C(CC(OC)C23)(OC(=O)C)C4C5OC(=O)c6ccccc6 DPMGVDIWDTYPMP-UHFFFAOYSA-N 0.000 description 5
- FIDOCHXHMJHKRW-GKVQVCCJSA-N hypaconitine Chemical compound O([C@H]1[C@]2(O)C[C@H]3[C@]45[C@@H](OC)CC[C@@]6([C@H]4[C@@H](OC)[C@H]([C@@](OC(C)=O)([C@H]31)[C@@H](O)[C@H]2OC)[C@H]5N(C)C6)COC)C(=O)C1=CC=CC=C1 FIDOCHXHMJHKRW-GKVQVCCJSA-N 0.000 description 5
- GQRPJUIKGLHLLN-VSTHTWNCSA-N mesaconine Chemical compound COC[C@]12CN(C)C3[C@@H]4[C@H](OC)[C@H]1[C@]3([C@@H]1C[C@@]3(O)[C@H](O)[C@@H]1[C@]4(O)[C@@H](O)[C@@H]3OC)[C@H](C[C@H]2O)OC GQRPJUIKGLHLLN-VSTHTWNCSA-N 0.000 description 5
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 description 4
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- 230000005180 public health Effects 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- ONBIUAZBGHXJDM-UHFFFAOYSA-J bismuth;potassium;tetraiodide Chemical compound [K+].[I-].[I-].[I-].[I-].[Bi+3] ONBIUAZBGHXJDM-UHFFFAOYSA-J 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 description 1
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Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention discloses a method for controlling quality of a medicine for treating rheumatism and apoplexy diseases. A maker component content measurement method for a Chinese medicine is combined with a thin-layer chromatography detection method, so the aim of controlling and evaluating the quality of a Chinese medicinal preparation is fulfilled. The method is easy and practicable, accurate and reliable, and high in accuracy and has very high practical value. By adoption of the method, the quality control over relative products can be improved greatly, so the quality of the products can be guaranteed, and the requirements of parties concerned on quality control over the medicine for treating rheumatism and apoplexy diseases can be met.
Description
Technical field
The present invention relates to derive from the quality control of the pharmaceutical products of plant material, be specifically related to a kind of method of quality control for the treatment of the medicine of rheumatism, apoplexy diseases.
Background technology
The Chinese medicine preparation of the medicine for the treatment of rheumatism, apoplexy diseases, as product Sanwu glue, the Sanwu capsule and pill of Yunnan Golden Crow black powder pharmaceutical Co. Ltd, this kind is recorded in " the 20 of Drug Standard of Ministry of Public Health of the Peoples Republic of China-Traditional Chinese medicine historical preparation ".
The Chinese medicine preparation of described treatment rheumatism, the medicine of apoplexy diseases is to be prepared by the raw material of following weight proportion:
Radix Aconiti Kusnezoffii 900g Radix Aconiti 600g fleece-flower root 450g
The raw rhizoma typhonii 300g of monkshood (tag) 150g frankincense 30g
Rock sugar 90g Fresh Ungula Sus domestica 500g.
Sanwu glue is according to Chinese medicine nomenclature principle, by Radix Aconiti Kusnezoffii, Radix Aconiti and the fleece-flower root three taste medicinal material called afters " Sanwu " in prescription, because auxiliary material Fresh Ungula Sus domestica in prescription has the effect of plastic, the medicinal extract of making has the character of jelly, the type of preparation of making belongs to jelly, so called after " Sanwu glue ".
Described Chinese medicine preparation can be to take Sanwu glue, Sanwu capsule and pill or the product of other formulation that above-mentioned active component makes as raw material.CN1265309A discloses the preparation method of this Chinese medicine preparation, its mature preparation process, and determined curative effect, safe and reliable.
Current method of quality control mainly comprises aconitine limit and volatile alkaline substance, as the method for regulation in " the 20 of Drug Standard of Ministry of Public Health of the Peoples Republic of China-Traditional Chinese medicine historical preparation ".Aconitine limit detection method is that precision takes 5g, puts in tool plug conical flask, adds ammonia solution 5ml, stir pulping, add zeyssatite 8g, grind well, add chloroform 60ml, close plug, placement is spent the night, ultrasonic processing 15 minutes, filters, chloroform 20ml washing for filter residue and filter, combined chloroform liquid, puts evaporate to dryness in water-bath, continues to steam 15 minutes, residue makes to dissolve with absolute ethyl alcohol 2ml, as need testing solution.Separately get aconitine reference substance, add absolute ethyl alcohol and make every 1ml containing the solution of 2mg, in contrast product solution.According to thin-layered chromatography (appendix VI B), test, draw need testing solution 10 μ l, reference substance solution 5 μ l, put respectively in same and take on the silica gel g thin-layer plate that sodium carboxymethyl cellulose is bonding agent, cyclohexane-the diethylamine (8: 2) of take is developping agent, launch, take out, dry, spray is with rare bismuth potassium iodide test solution.In test sample chromatogram, with the corresponding position of reference substance chromatogram on the spot that occurs should be less than the spot of reference substance or not occur spot.
Clinical practice proves, only detects above-mentioned project and can not meet the requirement that the quality of the pharmaceutical preparations is controlled.Therefore in order better to control the quality of Chinese medicine preparation of the medicine of described treatment rheumatism, apoplexy diseases, for the active component of the Chinese medicine preparation of the medicine of described rheumatism, apoplexy diseases is effectively monitored, a kind of new, more reasonable, science, effective method of quality control is extremely expected to propose by relevant department, to meet the needs of pharmaceutical field and clinical practice.
Summary of the invention
The technical issues that need to address of the present invention are the method for quality control that disclose a kind of Chinese medicine preparation of medicine for the treatment of rheumatism, apoplexy diseases, to overcome the existing above-mentioned defect of existing method, satisfy the demand.
The Chinese medicine preparation of described rheumatism, the medicine of apoplexy diseases is to be prepared by 8 above-mentioned taste raw materials, as the whole index components content to preparation are measured, obviously be unfavorable for actual suitability for industrialized production, applicant thinks, must selectively detect it, for this reason, applicant has proposed following technical scheme:
(1) the index components content assaying method of the fleece-flower root;
(2) diester-type alkaloids content assaying method in product;
(3) thin-layered chromatography detection method of frankincense;
(4) thin-layered chromatography detection method of the fleece-flower root;
(5) volatile alkaline substance detection method.
Why the present invention selects technical scheme as above, main because use these technical schemes, the Chinese medicine preparation that can treat the medicine of rheumatism, apoplexy diseases to this carries out quality control, confirm whether to contain in said preparation the medicinal material of technical scheme demarcation, and combine by least two kinds of above technical schemes, in method of quality control, assert more than two and two qualifying points, improve the method for quality control of preparation and better the quality of the pharmaceutical preparations is controlled.
Best-of-breed technology scheme is that above five kinds of all technical schemes are combined, and jointly the quality of the pharmaceutical preparations is controlled, and can from 5 reference mark, carry out quality monitoring to preparation.
Wherein:
(1) the index components content assaying method of the fleece-flower root
Chromatographic condition and system suitability be take octadecylsilane chemically bonded silica as filling agent; The acetonitrile-water (20: 80) of take is mobile phase; Detection wavelength is 320nm.Number of theoretical plate calculates and should be not less than 3000 by 2,3,5,4 '-tetrahydroxystilbene-2-O-β-D-Glucose glycosides peak.
The preparation precision of reference substance solution takes 2,3, and 5,4 '-tetrahydroxystilbene-2-O-β-D-Glucose glycosides reference substance is appropriate, adds Diluted Alcohol and makes every 1ml containing the solution of 0.1mg, obtains.
This product porphyrize is got in the preparation of need testing solution, gets about 0.4g, accurately weighed, puts in tool plug conical flask, add sherwood oil (30～60 ℃) 15ml, close plug, ultrasonic processing 5 minutes, standing, discard sherwood oil liquid, then same treatment once, residue tepor volatilizes, and precision adds Diluted Alcohol 25ml, close plug, weighed weight, ultrasonic processing (power 250W, frequency 25kHz) 15 minutes, let cool, more weighed weight, with Diluted Alcohol, supply the weight of less loss, shake up, filter, get subsequent filtrate, obtain.
Determination method is accurate reference substance solution and each 10 μ l of need testing solution of drawing respectively, and injection liquid chromatography, measures, and obtains.
(2) diester-type alkaloids content assaying method in product
Chromatographic condition and system suitability be take octadecyl silane as filling agent; 0.04mol/L triethylamine (phosphoric acid regulates the PH=3.0)-methyl alcohol (60: 40) of take is mobile phase; Detect wavelength: 235nm; Column temperature: 40 ℃.Number of theoretical plate calculates and should be not less than 3000 by aconitine peak.
It is appropriate, accurately weighed that mesaconine, Hypaconitine and aconitine reference substance are got in the preparation of reference substance solution, adds 10% methanol solution (phosphoric acid is adjusted PH=2.0) and make every 1ml respectively containing the mixed solution of 0.05mg, obtains.
This product porphyrize is got in the preparation of need testing solution, and precision takes 5g, adds sherwood oil (30～60 ℃) 15ml, ultrasonic processing 5 minutes, standing, supernatant inclines, once, tepor volatilizes same treatment again, adds ammonia solution 5ml, mix, the 30ml that adds diethyl ether, close plug, ultrasonic processing (25 ℃ of water temperatures are following) 15 minutes, placement is spent the night, and divides and gets ether solution.The residue 30ml that adds diethyl ether, ultrasonic processing (25 ℃ of water temperatures are following) 15 minutes, minute gets ether solution.Add diethyl ether agitator treating 3 times of residue, each 15ml, merges ether solution, 40 ℃ of following evaporates to dryness, residue adds 10% methanol solution (phosphoric acid is adjusted PH=2.0) makes to be dissolved into 5ml, shakes up, and obtains.
Determination method is accurate reference substance solution and each 20 μ l of need testing solution of drawing respectively, and injection liquid chromatography, measures, and obtains.
(3) thin-layered chromatography detection method of frankincense
Get this product porphyrize, take 10g, put in tool plug conical flask, the 60ml that adds diethyl ether, ultrasonic processing 15 minutes, divides and gets ether solution, filters, and filtrate tepor volatilizes, and residue adds absolute ethyl alcohol 1ml to be made to dissolve, as need testing solution.Get frankincense control medicinal material 0.25g, put in tool plug conical flask, the 30ml that adds diethyl ether, close plug, ultrasonic processing 15 minutes, filters, filtrate evaporate to dryness, residue makes to dissolve with absolute ethyl alcohol 1ml, in contrast medicinal material solution.According to thin-layered chromatography (appendix VI B), test, draw above-mentioned control medicinal material solution 2 μ l, need testing solution 6～10 μ l, put respectively in same and take on the silica gel g thin-layer plate that sodium carboxymethyl cellulose is bonding agent, sherwood oil (60～90 ℃)-benzene-ethyl acetate (10: 1.5: 1.5) of take are developping agent, launch, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid test solution, and 105 ℃ to be heated to spot colour developing clear.In test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the spot of aobvious same color.With this, judge in preparation, whether to contain frankincense.
(4) thin-layered chromatography detection method of the fleece-flower root
Get this product porphyrize, take 10g, put in tool plug conical flask, the 60ml that adds diethyl ether, ultrasonic processing 15 minutes, divides and gets ether solution, filters, and filtrate tepor volatilizes, and residue adds absolute ethyl alcohol 1ml to be made to dissolve, as need testing solution.Get fleece-flower root control medicinal material 0.25g, be made in the same way of control medicinal material solution.Get archen reference substance, add absolute ethyl alcohol and make every 1ml containing the solution of 0.5mg, in contrast product solution.According to thin-layered chromatography (appendix VI B), test, draw each 3 μ l of above-mentioned need testing solution 3～5 μ l, control medicinal material solution and reference substance solution, put respectively in same and take on the silica gel g thin-layer plate that sodium carboxymethyl cellulose is bonding agent, take normal hexane-ethyl acetate-methyl alcohol-formic acid (8: 2: 1: 0.2) be developping agent, launch, take out, dry, put under ultraviolet lamp (365nm) and inspect.In test sample chromatogram, with control medicinal material chromatogram and the corresponding position of reference substance chromatogram on, the fluorescence spot of aobvious same color; Put in ammonia steam smoked after, under daylight, inspect, spot becomes pale red.With this, judge in preparation, whether to contain the fleece-flower root.
(5) volatile alkaline substance detection method
Get this product porphyrize, precision takes 0.5g, puts in 100ml round-bottomed flask, add water 10ml and make to dissolve, add 0.10g magnesia powder, rapid close plug, mix, pass into water vapor and distill, with 2% BAS 10ml, methylate is red-and to mix 5 of indicator solutions be receiving liquid to bromcresol green, from ooze the 1st while condensing the globule, distill and stop for 15 minutes, distillate, according to n2 method (appendix IX L bis-methods) titration, obtains.In 100g sample, the content of volatile alkaline substance, in nitrogen (N), must not be crossed 60mg
The present invention adopts the index components assay of Chinese medicine to combine with thin-layered chromatography detection method, reaches the object of controlling and evaluating this Chinese medicine preparation quality.Method provided by the present invention is compared for this Chinese medicine initial quality control method, more scientific and reasonable, effective.From operation, method provided by the invention is simple, accurately and reliably.Degree of accuracy is high, has very high practical value.Because the present invention has adopted above-mentioned method, therefore, can greatly improve the quality control of related products, to guarantee the quality of product, can meet the needs of the parties concerned to the quality monitoring of the medicine for the treatment of rheumatism, apoplexy diseases.
Embodiment
Embodiment 1
The check of Sanwu glue
Test sample: the jelly that adopts 8 above-mentioned taste medicine systems to prepare, Yunnan Golden Crow black powder pharmaceutical Co. Ltd produces.The specific operation process of the method for inspection of Sanwu glue is as follows:
(1) the index components content assaying method of the fleece-flower root
Chromatographic condition and system suitability be take octadecylsilane chemically bonded silica as filling agent; The acetonitrile-water (20: 80) of take is mobile phase; Detection wavelength is 320nm.Number of theoretical plate calculates and should be not less than 3000 by 2,3,5,4 '-tetrahydroxystilbene-2-O-β-D-Glucose glycosides peak.
The preparation precision of reference substance solution takes 2,3, and 5,4 '-tetrahydroxystilbene-2-O-β-D-Glucose glycosides reference substance is appropriate, adds Diluted Alcohol and makes every 1ml containing the solution of 0.1mg, obtains.
This product porphyrize is got in the preparation of need testing solution, gets about 0.4g, accurately weighed, puts in tool plug conical flask, add sherwood oil (30～60 ℃) 15ml, close plug, ultrasonic processing 5 minutes, standing, discard sherwood oil liquid, then same treatment once, residue tepor volatilizes, and precision adds Diluted Alcohol 25ml, close plug, weighed weight, ultrasonic processing (power 250W, frequency 25kHz) 15 minutes, let cool, more weighed weight, with Diluted Alcohol, supply the weight of less loss, shake up, filter, get subsequent filtrate, obtain.
Determination method is accurate reference substance solution and each 10 μ l of need testing solution of drawing respectively, and injection liquid chromatography, measures, and obtains.
Testing result is as follows: in Sanwu glue, every 1g contains the fleece-flower root with 2,3,5,4 '-tetrahydroxystilbene-2-O-β-D-Glucose glycosides (C
20h
32o
9) meter, 4.05mg/g.
(2) diester-type alkaloids content assaying method in product
Chromatographic condition and system suitability be take octadecyl silane as filling agent; 0.04mol/L triethylamine (phosphoric acid regulates the PH=3.0)-methyl alcohol (60: 40) of take is mobile phase; Detect wavelength: 235nm; Column temperature: 40 ℃.Number of theoretical plate calculates and should be not less than 3000 by aconitine peak.
It is appropriate, accurately weighed that mesaconine, Hypaconitine and aconitine reference substance are got in the preparation of reference substance solution, adds 10% methanol solution (phosphoric acid is adjusted PH=2.0) and make every 1ml respectively containing the mixed solution of 0.05mg, obtains.
This product porphyrize is got in the preparation of need testing solution, and precision takes 5g, adds sherwood oil (30～60 ℃) 15ml, ultrasonic processing 5 minutes, standing, supernatant inclines, once, tepor volatilizes same treatment again, adds ammonia solution 5ml, mix, the 30ml that adds diethyl ether, close plug, ultrasonic processing (25 ℃ of water temperatures are following) 15 minutes, placement is spent the night, and divides and gets ether solution.The residue 30ml that adds diethyl ether, ultrasonic processing (25 ℃ of water temperatures are following) 15 minutes, minute gets ether solution.Add diethyl ether agitator treating 3 times of residue, each 15ml, merges ether solution, 40 ℃ of following evaporates to dryness, residue adds 10% methanol solution (phosphoric acid is adjusted PH=2.0) makes to be dissolved into 5ml, shakes up, and obtains.
Determination method is accurate reference substance solution and each 20 μ l of need testing solution of drawing respectively, and injection liquid chromatography, measures, and obtains.
Testing result is as follows: in Sanwu glue, contain diester-type alkaloids with mesaconine (C
33h
45nO
11), Hypaconitine (C
33h
45nO
10) and aconitine (C
34h
47nO
11) total amount meter, be 0.015%.
(3) thin-layered chromatography detection method of frankincense
Get this product porphyrize, take 10g, put in tool plug conical flask, the 60ml that adds diethyl ether, ultrasonic processing 15 minutes, divides and gets ether solution, filters, and filtrate tepor volatilizes, and residue adds absolute ethyl alcohol 1ml to be made to dissolve, as need testing solution.Get frankincense control medicinal material 0.25g, put in tool plug conical flask, the 30ml that adds diethyl ether, close plug, ultrasonic processing 15 minutes, filters, filtrate evaporate to dryness, residue makes to dissolve with absolute ethyl alcohol 1ml, in contrast medicinal material solution.According to thin-layered chromatography (appendix VI B), test, draw above-mentioned control medicinal material solution 2 μ l, need testing solution 6～10 μ l, put respectively in same and take on the silica gel g thin-layer plate that sodium carboxymethyl cellulose is bonding agent, sherwood oil (60～90 ℃)-benzene-ethyl acetate (10: 1.5: 1.5) of take are developping agent, launch, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid test solution, and 105 ℃ to be heated to spot colour developing clear.In test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the spot of aobvious same color.
(4) thin-layered chromatography detection method of the fleece-flower root
Get this product porphyrize, take 10g, put in tool plug conical flask, the 60ml that adds diethyl ether, ultrasonic processing 15 minutes, divides and gets ether solution, filters, and filtrate tepor volatilizes, and residue adds absolute ethyl alcohol 1ml to be made to dissolve, as need testing solution.Get fleece-flower root control medicinal material 0.25g, be made in the same way of control medicinal material solution.Get archen reference substance, add absolute ethyl alcohol and make every 1ml containing the solution of 0.5mg, in contrast product solution.According to thin-layered chromatography (appendix VI B), test, draw each 3 μ l of above-mentioned need testing solution 3～5 μ l, control medicinal material solution and reference substance solution, put respectively in same and take on the silica gel g thin-layer plate that sodium carboxymethyl cellulose is bonding agent, take normal hexane-ethyl acetate-methyl alcohol-formic acid (8: 2: 1: 0.2) be developping agent, launch, take out, dry, put under ultraviolet lamp (365nm) and inspect.In test sample chromatogram, with control medicinal material chromatogram and the corresponding position of reference substance chromatogram on, the fluorescence spot of aobvious same color; Put in ammonia steam smoked after, under daylight, inspect, spot becomes pale red.
(5) volatile alkaline substance detection method
Get this product porphyrize, precision takes 0.5g, puts in 100ml round-bottomed flask, add water 10ml and make to dissolve, add 0.10g magnesia powder, rapid close plug, mix, pass into water vapor and distill, with 2% BAS 10ml, methylate is red-and to mix 5 of indicator solutions be receiving liquid to bromcresol green, from ooze the 1st while condensing the globule, distill and stop for 15 minutes, distillate, according to n2 method (appendix IX L bis-methods) titration, obtains.In 100g sample, the content of volatile alkaline substance, in nitrogen (N), must not be crossed 100mg.
Testing result is as follows: 20.25mg/100g
Embodiment 2
The check of Sanwu capsule and pill
Test sample: the jelly that adopts 8 above-mentioned taste medicine systems to prepare, Yunnan Golden Crow black powder pharmaceutical Co. Ltd produces, and the specific operation process of the method for inspection of Sanwu glue is as follows:
(1) the index components content assaying method of the fleece-flower root
Chromatographic condition and system suitability be take octadecylsilane chemically bonded silica as filling agent; The acetonitrile-water (20: 80) of take is mobile phase; Detection wavelength is 320nm.Number of theoretical plate calculates and should be not less than 3000 by 2,3,5,4 '-tetrahydroxystilbene-2-O-β-D-Glucose glycosides peak.
The preparation precision of reference substance solution takes 2,3, and 5,4 '-tetrahydroxystilbene-2-O-β-D-Glucose glycosides reference substance is appropriate, adds Diluted Alcohol and makes every 1ml containing the solution of 0.1mg, obtains.
This product porphyrize is got in the preparation of need testing solution, gets about 0.4g, accurately weighed, puts in tool plug conical flask, add sherwood oil (30～60 ℃) 15ml, close plug, ultrasonic processing 5 minutes, standing, discard sherwood oil liquid, then same treatment once, residue tepor volatilizes, and precision adds Diluted Alcohol 25ml, close plug, weighed weight, ultrasonic processing (power 250W, frequency 25kHz) 15 minutes, let cool, more weighed weight, with Diluted Alcohol, supply the weight of less loss, shake up, filter, get subsequent filtrate, obtain.
Determination method is accurate reference substance solution and each 10 μ l of need testing solution of drawing respectively, and injection liquid chromatography, measures, and obtains.
Testing result is as follows: in Sanwu capsule and pill, every 1g contains the fleece-flower root with 2,3,5,4 '-tetrahydroxystilbene-2-O-β-D-Glucose glycosides (C
20h
22o
9) meter, 4.20mg/g.
(2) diester-type alkaloids content assaying method in product
Chromatographic condition and system suitability be take octadecyl silane as filling agent; 0.04mol/L triethylamine (phosphoric acid regulates the PH=3.0)-methyl alcohol (60: 40) of take is mobile phase; Detect wavelength: 235nm; Column temperature: 40 ℃.Number of theoretical plate calculates and should be not less than 3000 by aconitine peak.
It is appropriate, accurately weighed that mesaconine, Hypaconitine and aconitine reference substance are got in the preparation of reference substance solution, adds 10% methanol solution (phosphoric acid is adjusted PH=2.0) and make every 1ml respectively containing the mixed solution of 0.05mg, obtains.
This product porphyrize is got in the preparation of need testing solution, and precision takes 5g, adds sherwood oil (30～60 ℃) 15ml, ultrasonic processing 5 minutes, standing, supernatant inclines, once, tepor volatilizes same treatment again, adds ammonia solution 5ml, mix, the 30ml that adds diethyl ether, close plug, ultrasonic processing (25 ℃ of water temperatures are following) 15 minutes, placement is spent the night, and divides and gets ether solution.The residue 30ml that adds diethyl ether, ultrasonic processing (25 ℃ of water temperatures are following) 15 minutes, minute gets ether solution.Add diethyl ether agitator treating 3 times of residue, each 15ml, merges ether solution, 40 ℃ of following evaporates to dryness, residue adds 10% methanol solution (phosphoric acid is adjusted PH=2.0) makes to be dissolved into 5ml, shakes up, and obtains.
Determination method is accurate reference substance solution and each 20 μ l of need testing solution of drawing respectively, and injection liquid chromatography, measures, and obtains.
Testing result is as follows: in Sanwu glue, contain diester-type alkaloids with mesaconine (C
33h
45nO
11), Hypaconitine (C
33h
45nO
10) and aconitine (C
34h
47nO
11) total amount meter, be 0.010%.
(3) thin-layered chromatography detection method of frankincense
Get this product porphyrize, take 10g, put in tool plug conical flask, the 60ml that adds diethyl ether, ultrasonic processing 15 minutes, divides and gets ether solution, filters, and filtrate tepor volatilizes, and residue adds absolute ethyl alcohol 1ml to be made to dissolve, as need testing solution.Get frankincense control medicinal material 0.25g, put in tool plug conical flask, the 30ml that adds diethyl ether, close plug, ultrasonic processing 15 minutes, filters, filtrate evaporate to dryness, residue makes to dissolve with absolute ethyl alcohol 1ml, in contrast medicinal material solution.According to thin-layered chromatography (appendix VI B), test, draw above-mentioned control medicinal material solution 2 μ l, need testing solution 6～10 μ l, put respectively in same and take on the silica gel g thin-layer plate that sodium carboxymethyl cellulose is bonding agent, sherwood oil (60～90 ℃)-benzene-ethyl acetate (10: 1.5: 1.5) of take are developping agent, launch, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid test solution, and 105 ℃ to be heated to spot colour developing clear.In test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the spot of aobvious same color.
(4) thin-layered chromatography detection method of the fleece-flower root
Get this product porphyrize, take 10g, put in tool plug conical flask, the 60ml that adds diethyl ether, ultrasonic processing 15 minutes, divides and gets ether solution, filters, and filtrate tepor volatilizes, and residue adds absolute ethyl alcohol 1ml to be made to dissolve, as need testing solution.Get fleece-flower root control medicinal material 0.25g, be made in the same way of control medicinal material solution.Get archen reference substance, add absolute ethyl alcohol and make every 1ml containing the solution of 0.5mg, in contrast product solution.According to thin-layered chromatography (appendix VI B), test, draw each 3 μ l of above-mentioned need testing solution 3～5 μ l, control medicinal material solution and reference substance solution, put respectively in same and take on the silica gel g thin-layer plate that sodium carboxymethyl cellulose is bonding agent, take normal hexane-ethyl acetate-methyl alcohol-formic acid (8: 2: 1: 0.2) be developping agent, launch, take out, dry, put under ultraviolet lamp (365nm) and inspect.In test sample chromatogram, with control medicinal material chromatogram and the corresponding position of reference substance chromatogram on, the fluorescence spot of aobvious same color; Put in ammonia steam smoked after, under daylight, inspect, spot becomes pale red.
(5) volatile alkaline substance detection method
Get this product porphyrize, precision takes 0.5g, puts in 100ml round-bottomed flask, add water 10ml and make to dissolve, add 0.10g magnesia powder, rapid close plug, mix, pass into water vapor and distill, with 2% BAS 10ml, methylate is red-and to mix 5 of indicator solutions be receiving liquid to bromcresol green, from ooze the 1st while condensing the globule, distill and stop for 15 minutes, distillate, according to n2 method (appendix IX L bis-methods) titration, obtains.In 100g sample, the content of volatile alkaline substance, in nitrogen (N), must not be crossed 60mg.
Testing result is as follows: 18.15mg/100g
Embodiment 3
Adopt the method for Selection and Constitute, choose any a collection of Sanwu glue, Sanwu capsule and pill detects, array mode see the following form (method of quality control that in table, √ representative is chosen, * represent unchecked method of quality control):
Result shows
Upper table has been arranged out 2-5 all in a quality inspection method of the present invention Combination of Methods, chooses wherein combination in any and all can carry out quality control for Sanwu glue (ball).
Claims (2)
1. a detection method for the treatment of the medicine of rheumatism, apoplexy diseases, is characterized in that, the Chinese medicine preparation of described medicine is prepared by following active component weight proportion raw material:
Radix Aconiti Kusnezoffii 900g Radix Aconiti 600g fleece-flower root 450g
The raw rhizoma typhonii 300g of monkshood 150g frankincense 30g
Rock sugar 90g Fresh Ungula Sus domestica 500g;
Described Chinese medicine preparation is Sanwu glue;
Comprise following checking procedure:
(1) the index components assay of the fleece-flower root;
(2) diester-type alkaloids assay in product;
(3) thin-layer chromatography of frankincense detects;
(4) thin-layer chromatography of the fleece-flower root detects;
(5) volatile alkaline substance detects;
Described fleece-flower root index components assay is: with 2,3, and 5,4 '-tetrahydroxystilbene-2-O-β-D-Glucose glycosides C
20h
22o
9for content, control index, adopt high effective liquid chromatography for measuring, its chromatographic condition is filling agent for adopting octadecylsilane chemically bonded silica, and the acetonitrile-water that the ratio of take is 20:80 is mobile phase, and detection wavelength is 320nm; Number of theoretical plate calculates and should be not less than 3000 by 2,3,5,4 '-tetrahydroxystilbene-2-O-β-D-Glucose glycosides peak;
Described diester-type alkaloids index assay is: take octadecyl silane as filling agent; 0.04mol/L triethylamine-methyl alcohol that the ratio of take is 60:40 is mobile phase, and wherein said triethylamine regulates pH=3.0 with phosphoric acid; Detect wavelength: 235nm; Column temperature: 40 ℃, number of theoretical plate calculates and should be not less than 3000 by aconitine peak;
The thin-layer chromatography of described frankincense detects: by the method for frankincense control medicinal material reference, its chromatographic condition is: the silica gel g thin-layer plate that the sodium carboxymethyl cellulose of take is bonding agent is chromatoplate, sherwood oil-benzene-ethyl acetate that the ratio of take under 60～90 ℃ of conditions is 10:1.5:1.5 is developping agent, launch, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid test solution, and 105 ℃ to be heated to spot colour developing clear; In comparison test sample chromatogram, with control medicinal material chromatogram, on corresponding position, whether show the spot of same color, with this, judge whether to contain frankincense medicinal material;
The thin-layer chromatography of the described fleece-flower root detects: by the method for fleece-flower root control medicinal material reference, its chromatographic condition is: the silica gel g thin-layer plate that the sodium carboxymethyl cellulose of take is bonding agent is chromatoplate, normal hexane-ethyl acetate-methyl alcohol-formic acid that the ratio of take is 8:2:1:0.2 is developping agent, launch, take out, dry, put under 365nm ultraviolet lamp and inspect, relatively whether test sample chromatogram and control medicinal material chromatogram, on corresponding position, show the fluorescence spot of same color; Put in ammonia steam smoked after, under daylight, inspect, spot becomes pale red, with this, judges whether to contain fleece-flower root medicinal material;
Described volatile alkaline substance detects: precision takes 0.5g, put in 100ml round-bottomed flask, adding water l0ml makes to dissolve, add 0.10g magnesia powder, rapid close plug, mix, pass into water vapor and distill, with 2% BAS 10ml, methylate is red-and to mix 5 of indicator solutions be receiving liquid to bromcresol green, from ooze the 1st while condensing the globule, distill and stop for 15 minutes, distillate, according to the n2 method titration in appendix IX L bis-methods, obtains, in 100g sample, the content of volatile alkaline substance is in nitrogen (N), and Sanwu glue must not be crossed 100mg.
2. a kind of detection method for the treatment of the medicine of rheumatism, apoplexy diseases according to claim 1, is characterized in that, described Sanwu glue is Sanwu capsule and pill; In 100g sample, the content of volatile alkaline substance is in nitrogen (N), and Sanwu capsule and pill must not be crossed 60mg.
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Address after: 654200 xianlongtan, east suburb of Huize County, Qujing City, Yunnan Province Patentee after: Yunnan Jinwu Pharmaceutical Co.,Ltd. Country or region after: China Address before: 654200 xianlongtan, east suburb of Huize County, Qujing City, Yunnan Province Patentee before: YUNNAN JINWUHEI PHARMACEUTICAL Co.,Ltd. Country or region before: China |