CN1588037A - <<XIAOKEWAN>> medicine quality control method for treating diabetes - Google Patents
<<XIAOKEWAN>> medicine quality control method for treating diabetes Download PDFInfo
- Publication number
- CN1588037A CN1588037A CN 200410051251 CN200410051251A CN1588037A CN 1588037 A CN1588037 A CN 1588037A CN 200410051251 CN200410051251 CN 200410051251 CN 200410051251 A CN200410051251 A CN 200410051251A CN 1588037 A CN1588037 A CN 1588037A
- Authority
- CN
- China
- Prior art keywords
- solution
- diabetes pill
- preparation
- add
- need testing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 206010012601 diabetes mellitus Diseases 0.000 title claims description 48
- 238000003908 quality control method Methods 0.000 title claims description 10
- 239000003814 drug Substances 0.000 title abstract description 18
- 229960004580 glibenclamide Drugs 0.000 claims abstract description 24
- ZNNLBTZKUZBEKO-UHFFFAOYSA-N glyburide Chemical compound COC1=CC=C(Cl)C=C1C(=O)NCCC1=CC=C(S(=O)(=O)NC(=O)NC2CCCCC2)C=C1 ZNNLBTZKUZBEKO-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 24
- 241001506371 Kadsura Species 0.000 claims abstract description 16
- 238000004587 chromatography analysis Methods 0.000 claims abstract description 13
- JEJFTTRHGBKKEI-OKILXGFUSA-N deoxyschizandrin Chemical compound C1[C@H](C)[C@H](C)CC2=CC(OC)=C(OC)C(OC)=C2C2=C1C=C(OC)C(OC)=C2OC JEJFTTRHGBKKEI-OKILXGFUSA-N 0.000 claims abstract description 7
- JEJFTTRHGBKKEI-UHFFFAOYSA-N deoxyschizandrin Natural products C1C(C)C(C)CC2=CC(OC)=C(OC)C(OC)=C2C2=C1C=C(OC)C(OC)=C2OC JEJFTTRHGBKKEI-UHFFFAOYSA-N 0.000 claims abstract description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 60
- 239000006187 pill Substances 0.000 claims description 44
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 22
- 238000012360 testing method Methods 0.000 claims description 22
- 238000002360 preparation method Methods 0.000 claims description 21
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 18
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 18
- 239000013558 reference substance Substances 0.000 claims description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 239000000706 filtrate Substances 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 9
- 239000009636 Huang Qi Substances 0.000 claims description 8
- QMNWISYXSJWHRY-YLNUDOOFSA-N astragaloside IV Chemical compound O1[C@H](C(C)(O)C)CC[C@]1(C)[C@@H]1[C@@]2(C)CC[C@]34C[C@]4(CC[C@H](O[C@H]4[C@@H]([C@@H](O)[C@H](O)CO4)O)C4(C)C)[C@H]4[C@@H](O[C@H]4[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O4)O)C[C@H]3[C@]2(C)C[C@@H]1O QMNWISYXSJWHRY-YLNUDOOFSA-N 0.000 claims description 7
- QMNWISYXSJWHRY-BCBPIKMJSA-N astragaloside IV Natural products CC(C)(O)[C@@H]1CC[C@@](C)(O1)[C@H]2[C@@H](O)C[C@@]3(C)[C@@H]4C[C@H](O[C@@H]5O[C@H](CO)[C@H](O)[C@@H](O)[C@H]5O)[C@H]6C(C)(C)[C@H](CC[C@@]67C[C@@]47CC[C@]23C)O[C@@H]8OC[C@@H](O)[C@H](O)[C@H]8O QMNWISYXSJWHRY-BCBPIKMJSA-N 0.000 claims description 7
- PFKIBRPYVNVMRU-UHFFFAOYSA-N cyclosieversioside F Natural products CC(C)(O)C1COC(C)(C1)C2C(O)CC3(C)C4CC(OC5OC(CO)C(O)C(O)C5O)C6C(C)(C)C(CCC67CC47CCC23C)OC8OCC(O)C(O)C8O PFKIBRPYVNVMRU-UHFFFAOYSA-N 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 6
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 6
- 235000019837 monoammonium phosphate Nutrition 0.000 claims description 6
- 239000013641 positive control Substances 0.000 claims description 6
- FYSHYFPJBONYCQ-UHFFFAOYSA-N schisanhenol Natural products C1C(C)C(C)CC2=CC(OC)=C(OC)C(OC)=C2C2=C1C=C(OC)C(OC)=C2O FYSHYFPJBONYCQ-UHFFFAOYSA-N 0.000 claims description 6
- 239000000377 silicon dioxide Substances 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- 238000005660 chlorination reaction Methods 0.000 claims description 4
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 3
- 239000003513 alkali Substances 0.000 claims description 3
- 239000000945 filler Substances 0.000 claims description 3
- 235000019253 formic acid Nutrition 0.000 claims description 3
- 239000006210 lotion Substances 0.000 claims description 3
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 claims description 3
- 229920006395 saturated elastomer Polymers 0.000 claims description 3
- 239000000741 silica gel Substances 0.000 claims description 3
- 229910002027 silica gel Inorganic materials 0.000 claims description 3
- 239000007921 spray Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 238000001514 detection method Methods 0.000 claims 1
- 238000004128 high performance liquid chromatography Methods 0.000 claims 1
- 229940079593 drug Drugs 0.000 abstract description 5
- 238000004809 thin layer chromatography Methods 0.000 abstract description 4
- 238000003556 assay Methods 0.000 abstract description 2
- 230000003178 anti-diabetic effect Effects 0.000 abstract 3
- 241001061264 Astragalus Species 0.000 abstract 2
- 241000736075 Schisandra Species 0.000 abstract 2
- 235000008422 Schisandra chinensis Nutrition 0.000 abstract 2
- 235000006533 astragalus Nutrition 0.000 abstract 2
- 210000004233 talus Anatomy 0.000 abstract 2
- 239000003472 antidiabetic agent Substances 0.000 abstract 1
- 238000012207 quantitative assay Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 36
- 239000000047 product Substances 0.000 description 6
- 239000007791 liquid phase Substances 0.000 description 4
- 235000002722 Dioscorea batatas Nutrition 0.000 description 2
- 235000006536 Dioscorea esculenta Nutrition 0.000 description 2
- 240000001811 Dioscorea oppositifolia Species 0.000 description 2
- 235000003416 Dioscorea oppositifolia Nutrition 0.000 description 2
- 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 description 2
- 239000007767 bonding agent Substances 0.000 description 2
- 239000001768 carboxy methyl cellulose Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 description 2
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 description 2
- 239000011550 stock solution Substances 0.000 description 2
- 101100117236 Drosophila melanogaster speck gene Proteins 0.000 description 1
- 244000046146 Pueraria lobata Species 0.000 description 1
- 235000010575 Pueraria lobata Nutrition 0.000 description 1
- 241000405414 Rehmannia Species 0.000 description 1
- 241000218989 Trichosanthes Species 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 238000012850 discrimination method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 230000003760 hair shine Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000005180 public health Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
Landscapes
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention provides a quantity control method for a kind of antidiabetic, which belongs to medication field. Concretely, It relates to the quantity control method of the combination of the Traditional Chinese medicine with the Westen medicine. It adds the following method to the original quantity control standard. (1): adopting thin layer chromatography, contrasting to to identify if the antidiabetics contain astragalus. (2) adopting thin layer chromatography to comparing the Wuweizisu A to schisandra chinenis positive to indetify if the antidiabetics contain kadsura longepedunculata (3) Adopting high performance chromatography to assay the percentage content of the weigh of the glyburide is 0.07%-0.11%. The invention improves the quantity control technique of the antidiaetics, increase the identification method of if the abtidiabetics with high sepcificity contain astragalus and schisandra and can make a quantitative assay for the glyburide content, so as to control the quantity of the products to secure the safety to human pharmacy.
Description
Technical field
The invention belongs to field of medicaments, in being specifically related to, the method for quality control of western drug composition.
Background technology
A kind of medicine for the treatment of diabetes, diabetes pill are to go on the market for many years, the medicine that the clinical practice curative effect is sure, and be the medicine that has recorded in China national Ministry of Public Health ministerial standard.Diabetes pill is by the water extract of the Chinese crude drug root of kudzu vine, glutinous rehmannia, root of Chinese trichosanthes, corn stigma and the Radix Astragali, kadsura longepedunculata, the powder of Chinese yam and the compound that synthetic drug (being commonly called as Western medicine) glibenclamide is made, and prepares the common process preparation of pill by Chinese medicine.The quality of control final products is to carry out by ministry of Health of China ministerial standard MS-B-3476-98, and the microscopical identification of the Radix Astragali, kadsura longepedunculata, Chinese yam is only arranged in the standard, specificity is relatively poor, check the limit of glibenclamide with the size of thin-layered chromatography observation speck area, this thin-layer method is measured limit, the factor of operating process influence is a lot, the subjective factor influence of observing spot size is very big, can not reflect the content of glibenclamide in the product exactly, so be necessary further to study the method for quality control of this kind.
Summary of the invention
The objective of the invention is to improve the method for the quality control of a kind of treatment diabetes medicament " diabetes pill ".
Technical scheme of the present invention is: the discriminating item in the proper mass control criterion has increased (1) employing thin-layered chromatography, and the Astragaloside IV positive control is differentiated in the diabetes pill and contained the Radix Astragali; (2) adopt thin-layered chromatography, schizandrin A and kadsura longepedunculata positive control are differentiated in the diabetes pill and are contained kadsura longepedunculata; (3) adopting the high efficiency chromatography method to measure the percent by weight that contains glibenclamide in the diabetes pill is 0.07～0.11%, is equivalent to 70～110% of labelled amount.
Make positive control with Astragaloside IV and differentiate that the preferable thin-layer chromatography condition that contains the Radix Astragali in the diabetes pill is: the preparation of (1) need testing solution: get diabetes pill and pulverize, add dissolve with methanol, filter, get the filtrate evaporate to dryness, add the normal butyl alcohol dissolving, filter, filtrate is washed with sodium hydroxide solution, discard alkali lye, with the saturated water washing of normal butyl alcohol, discard water lotion, the evaporate to dryness normal butyl alcohol, residue adds dissolve with methanol, is need testing solution;
(2) preparation of reference substance solution: get Astragaloside IV and add dissolve with methanol, make the solution of 1mg/ml;
(3) thin layer preparation: point sample is in silica gel g thin-layer plate, and with chloroform: ethyl acetate: methyl alcohol: water is 20: 40: 22: 10 make developping agent, spray with behind 10% ethanol solution of sulfuric acid in the colour developing down of 365nm ultraviolet light.
Make positive control with schizandrin A and kadsura longepedunculata and differentiate that the preferable thin-layer chromatography condition that contains kadsura longepedunculata in the diabetes pill is: the preparation of (1) need testing solution: get diabetes pill and pulverize, add the chloroform dissolving, filter, get the filtrate evaporate to dryness, add the chloroform dissolving, be need testing solution;
(2) preparation of reference substance solution: get schizandrin A and add the chloroform dissolving, make the solution of 1mg/ml; Get the kadsura longepedunculata medicinal material, chlorination copies the preparation method of need testing solution to make control medicinal material solution;
(3) thin layer preparation: point sample is in silica G F
254Thin layer plate, with sherwood oil: ethyl acetate: formic acid is that 20: 5: 1 upper solution is made developping agent, inspects under the 254nm ultraviolet light.
Measuring the preferable condition that contains glibenclamide content in the diabetes pill with the high efficiency chromatography method is:
(1) preparation of reference substance solution: get glibenclamide and add dissolve with methanol, make the solution that contains 0.025mg among the 1ml;
(2) preparation of need testing solution: get diabetes pill and add dissolve with methanol, press the inventory of diabetes pill and calculate, make 1ml and contain glibenclamide and be equivalent to 0.025mg suspending liquid, filter and get filtrate;
(3) chromatographic condition:
Chromatographic column: octadecylsilane chemically bonded silica is a filling agent.
Moving phase: volume ratio is the 0.05mol/L ammonium dihydrogen phosphate (ADP): the solution of acetonitrile=52: 48.
Detect wavelength: 228nm;
Theoretical cam curve: count 1000 by glibenclamide.
(4) determination method: get reference substance solution and need testing solution respectively and inject liquid chromatograph, measure, promptly.
This assay method is through the methodology checking, and negative sample is noiseless to measuring, and it is r=0.99998 that linear dependence is closed, and shows that glibenclamide is good linear relationship in 0.2724～0.8172 μ g scope.The recovery is 102% (n=5), and RSD is 1.32%.Measure 20 batches of diabetes pill samples with this method, the content results of glibenclamide is as follows:
The suitable labelled amount % of the suitable labelled amount % lot number of lot number content % content %
99090787 0.085 85 99090856 0.079 79
99090917 0.078 78 99010167 0.099 99
00060510 0.11 110 00040350 0.091 91
00040410 0.072 72 00040310 0.076 76
01080985 0.083 83 01091344 0.085 85
01111519 0.092 92 01060505 0.079 79
E00159 0.108 108 E00180 0.072 72
E00155 0.070 70 E00169 0.089 89
E00306 0.084 84 E00170 0.081 81
E00171 0.090 90 E00137 0.097 97
Good effect of the present invention is: the present invention has improved the method for the quality control of treatment diabetes medicament " diabetes pill ", increased the discrimination method that whether contains the Radix Astragali and kadsura longepedunculata in the strong diabetes pill of specificity, and can quantitative measurement the content of glibenclamide in the diabetes pill, more effectively control the quality of product, guarantee the drug safety of human body.
Description of drawings
Fig. 1. be the thin-layer chromatogram of the diabetes pill sample that compares with Astragaloside IV.
Fig. 2. be the thin-layer chromatogram of the diabetes pill sample that compares with kadsura longepedunculata.
Fig. 3. be the high-efficient liquid phase chromatogram of diabetes pill sample.
Fig. 4. be the high-efficient liquid phase chromatogram of glibenclamide sample.
Embodiment
Be described in detail technical scheme of the present invention below in conjunction with embodiment and accompanying drawing.
Embodiment: the lot number of getting Guangzhou Zhongyi Medicine Industry Co., Ltd's production is the diabetes pill of E00532.
1. contain the Radix Astragali in the discriminating diabetes pill:
Get diabetes pill 5.5g and pulverize, add methyl alcohol 30ml, sonicated 15 minutes, filter, the filtrate evaporate to dryness adds 95% normal butyl alcohol 30ml, sonicated 15 minutes filters, and filtrate is washed 3 times with 1% sodium hydroxide solution, each 20ml discards alkali lye, uses the saturated water washing of normal butyl alcohol 2 times, each 30ml discards water lotion, the evaporate to dryness normal butyl alcohol, residue adds methyl alcohol 1ml dissolving, is need testing solution; Other gets the Astragaloside IV reference substance, adds dissolve with methanol, makes the solution product solution in contrast that contains 1mg among the 1ml; Test according to the thin-layered chromatography in 2000 editions appendix of Chinese Pharmacopoeia, draw each 3 μ l of above-mentioned two kinds of solution, respectively point sample in same be the silica gel g thin-layer plate of bonding agent with the sodium carboxymethyl cellulose, with chloroform: ethyl acetate: methyl alcohol: water (20: 40: 22: 10) place the lower floor's solution that spends the night below 10 ℃ and make developping agent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, about 5 minutes of 90～100 ℃ of heating.In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the fluorescence spot of apparent same color under the daylight; The fluorescence spot of apparent same color under ultraviolet lamp (365nm), as shown in Figure 1.
2. contain kadsura longepedunculata in the discriminating diabetes pill:
Get diabetes pill 3g, pulverize, add chloroform 20ml, sonicated 30 minutes filters, and filtrate evaporate to dryness, residue add chloroform 2ml makes dissolving, as need testing solution; Other gets kadsura longepedunculata medicinal material 2g, and chlorination 20ml shines medicinal material solution in pairs with legal system; Get the schizandrin A reference substance again, chlorination is copied into the solution product solution in contrast that contains 1mg among every 1ml; Test according to the thin-layered chromatography in 2000 editions appendix of Chinese Pharmacopoeia, draw each 1 μ l of above-mentioned three kinds of solution, respectively point sample in same be on the silica GF254 thin layer plate of bonding agent with the sodium carboxymethyl cellulose, with sherwood oil (60-90 ℃): ethyl acetate: the upper solution of formic acid (20: 5: 1) is a developping agent, launch, take out, dry, put under the ultraviolet lamp (254nm) and inspect.In the test sample chromatogram, with control medicinal material chromatogram and the corresponding position of reference substance chromatogram on, show the spot of same color, as shown in Figure 2.
3. glibenclamide Determination on content in the diabetes pill: according to the high effective liquid chromatography for measuring in 2000 editions appendix of Chinese Pharmacopoeia.
(1) preparation of reference substance solution: the accurate title, decided glibenclamide reference substance 13.62mg, puts in the 50ml measuring bottle, adds dissolve with methanol to scale, shakes up, in contrast the product stock solution; Precision is measured reference substance stock solution 5ml and is put in the 50ml measuring bottle, adds methyl alcohol and is diluted to scale, shakes up, and promptly gets (27.24 μ g/ml).
(2) preparation of need testing solution: get diabetes pill 20 balls, porphyrize is got about 5 ball amounts (being equivalent to glibenclamide 1.25mg), the accurate title, decide, put in the 50ml measuring bottle, add methyl alcohol 40ml, sonicated 15 minutes, add methyl alcohol and be diluted to scale, shake up, filter, get subsequent filtrate, filter with miillpore filter (0.45 μ m), get filtrate promptly.
(3) chromatographic condition:
Chromatographic column: octadecylsilane chemically bonded silica is a filling agent
Moving phase: volume ratio is the 0.05mol/L ammonium dihydrogen phosphate (ADP): acetonitrile=52: 48;
Detect wavelength: 228nm;
Theoretical cam curve: count 1000 by glibenclamide.
(3) measure: accurate respectively reference substance solution and each 20 μ l of need testing solution of drawing, inject liquid chromatograph, measure, the result is shown in Fig. 3,4, and Fig. 3 is the high-efficient liquid phase chromatogram of diabetes pill sample.Fig. 4 is the high-efficient liquid phase chromatogram of glibenclamide sample.Result of calculation content is 0.097%, is equivalent to 97% of labelled amount.
Claims (4)
1, a kind of method of quality control of diabetes pill is characterized in that: (1) adopts thin-layered chromatography, and the Astragaloside IV positive control is differentiated in the diabetes pill and contained the Radix Astragali; (2) adopt thin-layered chromatography, schizandrin A and kadsura longepedunculata positive control are differentiated in the diabetes pill and are contained kadsura longepedunculata; (3) adopting the high efficiency chromatography method to measure the percent by weight that contains glibenclamide in the diabetes pill is 0.07～0.11%.
2, the method for quality control of diabetes pill according to claim 1 is characterized in that the thin-layered chromatography that contains the Radix Astragali in the said discriminating diabetes pill is:
(1) preparation of need testing solution: get diabetes pill and pulverize, add dissolve with methanol, filter, get the filtrate evaporate to dryness, add the normal butyl alcohol dissolving, filter, filtrate is washed with sodium hydroxide solution, discard alkali lye, with the saturated water washing of normal butyl alcohol, discard water lotion, the evaporate to dryness normal butyl alcohol, residue adds dissolve with methanol, is need testing solution;
(2) preparation of reference substance solution: get Astragaloside IV and add dissolve with methanol, be made for the solution of 1mg/ml;
(3) thin layer preparation: point sample is in silica gel g thin-layer plate, and with chloroform: ethyl acetate: methyl alcohol: water is 20: 40: 22: 10 make developping agent, spray with behind 10% ethanol solution of sulfuric acid in the colour developing down of 365nm ultraviolet light.
3, the method for quality control of diabetes pill according to claim 1 is characterized in that the thin-layered chromatography that contains kadsura longepedunculata in the said discriminating diabetes pill is:
(1) preparation of need testing solution: get diabetes pill and pulverize, add the chloroform dissolving, filter, get the filtrate evaporate to dryness, add the chloroform dissolving, be need testing solution;
(2) preparation of reference substance solution: get schizandrin A and add the chloroform dissolving, be made for the solution of 1mg/ml; Get the kadsura longepedunculata medicinal material, chlorination copies the preparation method of need testing solution to make control medicinal material solution;
(3) thin layer preparation: point sample is in silica G F
254Thin layer plate, with sherwood oil: ethyl acetate: formic acid is that 20: 5: 1 upper solution is made developping agent, inspects under the 254nm ultraviolet light.
4, the method for quality control of diabetes pill according to claim 1 is characterized in that the high performance liquid chromatography that contains glibenclamide in the said mensuration diabetes pill is:
(1) preparation of reference substance solution: get glibenclamide and add dissolve with methanol, make the solution that contains 0.025mg among the 1ml;
(2) preparation of need testing solution: get diabetes pill and add dissolve with methanol, press the inventory of diabetes pill and calculate, make 1ml and contain glibenclamide and be equivalent to 0.025mg suspending liquid, filter and get filtrate;
(3) chromatographic condition: with octadecylsilane chemically bonded silica is filling agent, 52: 48 0.05mol/L ammonium dihydrogen phosphate (ADP): acetonitrile solution is a moving phase, and the detection wavelength is 228nm, and theoretical cam curve counts 1000 by glibenclamide.
(4) determination method: get reference substance solution and need testing solution respectively and inject liquid chromatograph, measure, promptly.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410051251 CN1265196C (en) | 2004-08-30 | 2004-08-30 | <<Xiaokewan>> medicine quality control method for treating diabetes |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410051251 CN1265196C (en) | 2004-08-30 | 2004-08-30 | <<Xiaokewan>> medicine quality control method for treating diabetes |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1588037A true CN1588037A (en) | 2005-03-02 |
| CN1265196C CN1265196C (en) | 2006-07-19 |
Family
ID=34602415
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200410051251 Expired - Fee Related CN1265196C (en) | 2004-08-30 | 2004-08-30 | <<Xiaokewan>> medicine quality control method for treating diabetes |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1265196C (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1939472B (en) * | 2005-09-30 | 2010-12-01 | 北京奇源益德药物研究所 | Detection method of compound preparation for treating diabetes |
| CN1695713B (en) * | 2005-04-28 | 2012-02-08 | 成都中汇制药有限公司 | Medication for treating diabetes and preparation method and quality control method |
| CN102813840A (en) * | 2011-06-07 | 2012-12-12 | 广州中一药业有限公司 | Application of pharmaceutical composition in preparing medicines used for preventing and treating diabetic cardiomyopathy |
| CN104155371A (en) * | 2013-05-15 | 2014-11-19 | 广州白云山中一药业有限公司 | HPLC (High Performance Liquid Chromatography) fingerprint spectrum of Chinese herbal medicine compound preparation, namely fluid promoting pills, for treating diabetes and establishing method thereof |
| CN104991032A (en) * | 2015-07-23 | 2015-10-21 | 北京市药品检验所 | Thin layer chromatography for identifying doped kadsura longepedunculata in Chinese magnoliavine |
| CN105168195A (en) * | 2015-09-30 | 2015-12-23 | 浙江大学 | Drug composition containing metformin and schizandrin and used for treating diabetes |
| CN105403654A (en) * | 2015-12-11 | 2016-03-16 | 陇西保和堂药业有限责任公司 | Method raising radix astragali thin-layer chromatographic identification |
-
2004
- 2004-08-30 CN CN 200410051251 patent/CN1265196C/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1695713B (en) * | 2005-04-28 | 2012-02-08 | 成都中汇制药有限公司 | Medication for treating diabetes and preparation method and quality control method |
| CN1939472B (en) * | 2005-09-30 | 2010-12-01 | 北京奇源益德药物研究所 | Detection method of compound preparation for treating diabetes |
| CN102813840A (en) * | 2011-06-07 | 2012-12-12 | 广州中一药业有限公司 | Application of pharmaceutical composition in preparing medicines used for preventing and treating diabetic cardiomyopathy |
| CN102813840B (en) * | 2011-06-07 | 2014-08-06 | 广州白云山中一药业有限公司 | Application of pharmaceutical composition in preparing medicines used for preventing and treating diabetic cardiomyopathy |
| CN104155371A (en) * | 2013-05-15 | 2014-11-19 | 广州白云山中一药业有限公司 | HPLC (High Performance Liquid Chromatography) fingerprint spectrum of Chinese herbal medicine compound preparation, namely fluid promoting pills, for treating diabetes and establishing method thereof |
| CN104155371B (en) * | 2013-05-15 | 2015-09-30 | 广州白云山中一药业有限公司 | The method for building up of the compound Chinese medicinal preparation diabetes pill HPLC finger-print for the treatment of diabetes and HPLC finger-print thereof |
| CN104991032A (en) * | 2015-07-23 | 2015-10-21 | 北京市药品检验所 | Thin layer chromatography for identifying doped kadsura longepedunculata in Chinese magnoliavine |
| CN105168195A (en) * | 2015-09-30 | 2015-12-23 | 浙江大学 | Drug composition containing metformin and schizandrin and used for treating diabetes |
| CN105403654A (en) * | 2015-12-11 | 2016-03-16 | 陇西保和堂药业有限责任公司 | Method raising radix astragali thin-layer chromatographic identification |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1265196C (en) | 2006-07-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101049389A (en) | Method for controlling quality of granule preparation for treating chilly sensation type gastritis | |
| CN102269751B (en) | Detection method of Liuweinengxiao preparation | |
| CN102854281A (en) | Detection method of sugar-free strong loquat syrup | |
| CN1265196C (en) | <<Xiaokewan>> medicine quality control method for treating diabetes | |
| CN101444589A (en) | Quality standard of Fenqing Wulin Wan and inspection method thereof | |
| CN101829266A (en) | Method for detecting quality of bezoar snake bile bulbus fritilariae liquid | |
| CN102068600A (en) | Quality control method of venation relaxing and heart-nourishing pill as Chinese herbal preparation | |
| CN1739739A (en) | Chinese medicine prepn for treating ulcer and its prepn process and quality control method | |
| CN101327247A (en) | Senna formulation and quality control method | |
| CN100369614C (en) | Quality control method of compound gallblader freeflow solid preparation | |
| CN1785294A (en) | Quality control method of eucommia bark blood pressure lowering preparation for treating high blood pressure | |
| WO2009155755A1 (en) | Method for determining the contents of oligosaccharides in morinda officinalis | |
| CN1836673A (en) | Chinese medicinal soft capsule and method for preparing and controlling the quality of Chinese medicinal soft capsule | |
| CN1931343A (en) | Quality standard and inspection method for coronary heart disease treating medicine tablet of seven ingredients | |
| CN1369704A (en) | Method for testing quality of acanthopanax leaf | |
| CN1790013A (en) | Method for simultaneous determination of protocatechuic acid content and 5-hydroxymethyl furfural content in pulse-activating injection | |
| CN1679785A (en) | Chinese medicine preparation for treating inflammation preparation and quality control thereof | |
| CN1323676C (en) | Preparation method and quality control method of traditional Chinese medicine capsule for treating spleen and stomach weakness | |
| CN108267537A (en) | A kind of method of Cortex Phellodendri in discriminating shangqing pill | |
| CN101029890A (en) | Method for inspecting Chinese-medicinal preparation Kaiyinwan | |
| CN1308679C (en) | Quality detection method for oral liquid for curing infantile cough due to lung-heat | |
| CN101224259A (en) | Quality controlling method of compound south isatis root granules | |
| CN1846730A (en) | Chaihuang soft capsule preparing process and its quality control technology | |
| CN1814011A (en) | Medicine composition for treating upper respiratory tract inflammation, preparing method, quality control method and use | |
| CN100515445C (en) | Quality control method for traditional Chinese medicine preparation for treating generalized anxiety |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C56 | Change in the name or address of the patentee |
Owner name: GUANGZHOU BAIYUNSHAN ZHONGYI PHARMACEUTICAL CO., L Free format text: FORMER NAME: GUANGZHOU ZHONGYI PHARMACEUTICAL CO., LTD. |
|
| CP03 | Change of name, title or address |
Address after: 510530, No. 32, Po pan Road, Guangzhou, Guangdong, Luogang District Patentee after: GUANGZHOU BAIYUNSHAN ZHONGYI PHARMACEUTICAL Co.,Ltd. Address before: 510140 Guangdong city of Guangzhou province Liwan District Cong Gui Lu Cong GUI Street No. 63 Patentee before: GUANGZHOU ZHONGYI PHARMACEUTICAL Co.,Ltd. |
|
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20060719 |