CN101581710A - Method for detecting illegally added gliclazide in hypoglycemic Chinese patent medicament - Google Patents
Method for detecting illegally added gliclazide in hypoglycemic Chinese patent medicament Download PDFInfo
- Publication number
- CN101581710A CN101581710A CNA2009100401256A CN200910040125A CN101581710A CN 101581710 A CN101581710 A CN 101581710A CN A2009100401256 A CNA2009100401256 A CN A2009100401256A CN 200910040125 A CN200910040125 A CN 200910040125A CN 101581710 A CN101581710 A CN 101581710A
- Authority
- CN
- China
- Prior art keywords
- solution
- detection method
- gliclazide
- chemical reaction
- sample
- 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.)
- Pending
Links
- BOVGTQGAOIONJV-BETUJISGSA-N 1-[(3ar,6as)-3,3a,4,5,6,6a-hexahydro-1h-cyclopenta[c]pyrrol-2-yl]-3-(4-methylphenyl)sulfonylurea Chemical compound C1=CC(C)=CC=C1S(=O)(=O)NC(=O)NN1C[C@H]2CCC[C@H]2C1 BOVGTQGAOIONJV-BETUJISGSA-N 0.000 title claims abstract description 36
- 229960000346 gliclazide Drugs 0.000 title claims abstract description 36
- 230000002218 hypoglycaemic effect Effects 0.000 title claims abstract description 36
- 239000003814 drug Substances 0.000 title abstract description 30
- 238000000034 method Methods 0.000 title abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 32
- 239000000284 extract Substances 0.000 claims abstract description 29
- 238000001514 detection method Methods 0.000 claims abstract description 23
- 239000012085 test solution Substances 0.000 claims abstract description 17
- OXNIZHLAWKMVMX-UHFFFAOYSA-N picric acid Chemical compound OC1=C([N+]([O-])=O)C=C([N+]([O-])=O)C=C1[N+]([O-])=O OXNIZHLAWKMVMX-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229950002929 trinitrophenol Drugs 0.000 claims abstract description 13
- 239000003960 organic solvent Substances 0.000 claims abstract description 12
- 239000007864 aqueous solution Substances 0.000 claims abstract description 10
- 229920006395 saturated elastomer Polymers 0.000 claims abstract description 10
- 238000012545 processing Methods 0.000 claims abstract description 4
- 238000012360 testing method Methods 0.000 claims description 69
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 39
- 239000000243 solution Substances 0.000 claims description 34
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims description 27
- 238000001556 precipitation Methods 0.000 claims description 22
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 2
- WPHGSKGZRAQSGP-UHFFFAOYSA-N methylenecyclohexane Natural products C1CCCC2CC21 WPHGSKGZRAQSGP-UHFFFAOYSA-N 0.000 claims 1
- 239000002244 precipitate Substances 0.000 abstract description 5
- 229960003316 potassium mercuric iodide Drugs 0.000 abstract description 4
- 239000012670 alkaline solution Substances 0.000 abstract 2
- 238000000605 extraction Methods 0.000 abstract 1
- 238000001228 spectrum Methods 0.000 description 14
- 229940100389 Sulfonylurea Drugs 0.000 description 11
- 239000000843 powder Substances 0.000 description 10
- 239000002775 capsule Substances 0.000 description 9
- YROXIXLRRCOBKF-UHFFFAOYSA-N sulfonylurea Chemical class OC(=N)N=S(=O)=O YROXIXLRRCOBKF-UHFFFAOYSA-N 0.000 description 9
- LLJFMFZYVVLQKT-UHFFFAOYSA-N 1-cyclohexyl-3-[4-[2-(7-methoxy-4,4-dimethyl-1,3-dioxo-2-isoquinolinyl)ethyl]phenyl]sulfonylurea Chemical compound C=1C(OC)=CC=C(C(C2=O)(C)C)C=1C(=O)N2CCC(C=C1)=CC=C1S(=O)(=O)NC(=O)NC1CCCCC1 LLJFMFZYVVLQKT-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 4
- YASAKCUCGLMORW-UHFFFAOYSA-N Rosiglitazone Chemical compound C=1C=CC=NC=1N(C)CCOC(C=C1)=CC=C1CC1SC(=O)NC1=O YASAKCUCGLMORW-UHFFFAOYSA-N 0.000 description 4
- JLRGJRBPOGGCBT-UHFFFAOYSA-N Tolbutamide Chemical compound CCCCNC(=O)NS(=O)(=O)C1=CC=C(C)C=C1 JLRGJRBPOGGCBT-UHFFFAOYSA-N 0.000 description 4
- 238000012850 discrimination method Methods 0.000 description 4
- 229940079593 drug Drugs 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 4
- 229960004580 glibenclamide Drugs 0.000 description 4
- 229960004346 glimepiride Drugs 0.000 description 4
- WIGIZIANZCJQQY-RUCARUNLSA-N glimepiride Chemical compound O=C1C(CC)=C(C)CN1C(=O)NCCC1=CC=C(S(=O)(=O)NC(=O)N[C@@H]2CC[C@@H](C)CC2)C=C1 WIGIZIANZCJQQY-RUCARUNLSA-N 0.000 description 4
- ZJJXGWJIGJFDTL-UHFFFAOYSA-N glipizide Chemical compound C1=NC(C)=CN=C1C(=O)NCCC1=CC=C(S(=O)(=O)NC(=O)NC2CCCCC2)C=C1 ZJJXGWJIGJFDTL-UHFFFAOYSA-N 0.000 description 4
- 229960001381 glipizide Drugs 0.000 description 4
- 229960003468 gliquidone Drugs 0.000 description 4
- 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 description 4
- 229910000474 mercury oxide Inorganic materials 0.000 description 4
- UKWHYYKOEPRTIC-UHFFFAOYSA-N mercury(ii) oxide Chemical compound [Hg]=O UKWHYYKOEPRTIC-UHFFFAOYSA-N 0.000 description 4
- 239000000049 pigment Substances 0.000 description 4
- 230000035922 thirst Effects 0.000 description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 3
- 239000004202 carbamide Substances 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 206010012601 diabetes mellitus Diseases 0.000 description 3
- 239000006187 pill Substances 0.000 description 3
- 238000010791 quenching Methods 0.000 description 3
- 230000000171 quenching effect Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- FAEKWTJYAYMJKF-QHCPKHFHSA-N GlucoNorm Chemical compound C1=C(C(O)=O)C(OCC)=CC(CC(=O)N[C@@H](CC(C)C)C=2C(=CC=CC=2)N2CCCCC2)=C1 FAEKWTJYAYMJKF-QHCPKHFHSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 238000004587 chromatography analysis Methods 0.000 description 2
- 230000002950 deficient Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 238000004128 high performance liquid chromatography Methods 0.000 description 2
- 235000012054 meals Nutrition 0.000 description 2
- 239000012982 microporous membrane Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 2
- 229960002354 repaglinide Drugs 0.000 description 2
- 229960004586 rosiglitazone Drugs 0.000 description 2
- SUFUKZSWUHZXAV-BTJKTKAUSA-N rosiglitazone maleate Chemical compound [H+].[H+].[O-]C(=O)\C=C/C([O-])=O.C=1C=CC=NC=1N(C)CCOC(C=C1)=CC=C1CC1SC(=O)NC1=O SUFUKZSWUHZXAV-BTJKTKAUSA-N 0.000 description 2
- 229960003271 rosiglitazone maleate Drugs 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- QMNAQPMXDMLOLD-UHFFFAOYSA-N 6-methyl-4-oxo-5,6-dihydrothieno[2,3-b]thiopyran-2-sulfonamide Chemical compound S1C(C)CC(=O)C2=C1SC(S(N)(=O)=O)=C2 QMNAQPMXDMLOLD-UHFFFAOYSA-N 0.000 description 1
- 241000208340 Araliaceae Species 0.000 description 1
- 241001061264 Astragalus Species 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000009636 Huang Qi Substances 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 241000405414 Rehmannia Species 0.000 description 1
- 241001249696 Senna alexandrina Species 0.000 description 1
- PJANXHGTPQOBST-VAWYXSNFSA-N Stilbene Natural products C=1C=CC=CC=1/C=C/C1=CC=CC=C1 PJANXHGTPQOBST-VAWYXSNFSA-N 0.000 description 1
- 235000006533 astragalus Nutrition 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 229940126678 chinese medicines Drugs 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- -1 ketone hydrochloride Chemical class 0.000 description 1
- 229960004329 metformin hydrochloride Drugs 0.000 description 1
- OETHQSJEHLVLGH-UHFFFAOYSA-N metformin hydrochloride Chemical compound Cl.CN(C)C(=N)N=C(N)N OETHQSJEHLVLGH-UHFFFAOYSA-N 0.000 description 1
- XZWYZXLIPXDOLR-UHFFFAOYSA-N metformin hydrochloride Natural products CN(C)C(=N)NC(N)=N XZWYZXLIPXDOLR-UHFFFAOYSA-N 0.000 description 1
- BNYHRGTXRPWASY-UHFFFAOYSA-N nonylsulfonylurea Chemical compound CCCCCCCCCS(=O)(=O)NC(N)=O BNYHRGTXRPWASY-UHFFFAOYSA-N 0.000 description 1
- 229960001753 phenformin hydrochloride Drugs 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000009874 shenqi Substances 0.000 description 1
- 230000000192 social effect Effects 0.000 description 1
- PJANXHGTPQOBST-UHFFFAOYSA-N stilbene Chemical compound C=1C=CC=CC=1C=CC1=CC=CC=C1 PJANXHGTPQOBST-UHFFFAOYSA-N 0.000 description 1
- 235000021286 stilbenes Nutrition 0.000 description 1
- 210000004233 talus Anatomy 0.000 description 1
Landscapes
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention discloses a method for detecting illegally added gliclazide in a hypoglycemic Chinese patent medicament, which comprises the following steps: 1) processing a sample to be detected; 2) extracting the sample to be detected with an organic solvent to obtain an extract of the sample to be detected; 3) adding alkaline solution into the obtained extract to perform extraction and using an extract in an alkaline solution layer as test solution; 4) taking some test solution and dripping the test solution into saturated aqueous solution of trinitrophenol to perform a chemical reaction I; 5) dripping some test solution again and dripping the test solution into test solution of potassium mercuric iodide to perform a chemical reaction II; and 6) judging a detection result: if both the chemical reaction I and the chemical reaction II produce precipitates or turn turbid, the sample to be detected is determined to contain gliclazide. The method has the advantages of high speed, simplicity, flexibility, reliability, high specificity and the like and can be used in on-site supervision and check.
Description
Technical field
The present invention relates to illegal detection method of adding chemicals in a kind of Chinese patent drug, more particularly, the present invention relates to illegal detection method of adding the hypoglycemic chemicals in a kind of hypoglycemic pcm.
Background technology
Hypoglycemic pcm generally contains Chinese medicines such as genseng, the Radix Astragali and does not contain the hypoglycemic Western medicine, but illegally added the sulfonylurea Western medicine in the hypoglycemic pcm that has, as gliclazide, the patient has increased spinoff and risk after having taken the hypoglycemic pcm that is added with the hypoglycemic Western medicine under ignorant.At present, contained hypoglycemic Western medicine adopts thin-layered chromatography or high performance liquid chromatography to detect usually in the hypoglycemic pcm, but these methods need extra instrument and equipment, and length consuming time (thin-layered chromatography takes 1～2 hour, high performance liquid chromatography takes 3～4 hours), therefore at the scene during supervision and check and inapplicable.For this reason, set up a kind of fast, illegal detection method of adding the hypoglycemic chemicals in the hypoglycemic pcm of simple, sensitive, reliable, high specificity, have crucial social effect.
The present invention utilizes sulfonylurea hypoglycemic Western medicine---the physicochemical property of gliclazide, set up the detection method of contained gliclazide in a kind of brand-new hypoglycemic pcm, have advantages such as quick, simple and high specificity, overcome above-mentioned chromatographic various defectives.
Summary of the invention
The object of the present invention is to provide illegal detection method of adding gliclazide in a kind of hypoglycemic pcm.
The present invention is achieved by the following technical solutions: illegal detection method of adding gliclazide in a kind of hypoglycemic pcm may further comprise the steps:
1) processing of testing sample;
2) treated testing sample extracts with organic solvent, obtains the extract of testing sample;
3) add aqueous slkali in the resulting extract and extract, get aqueous slkali layer extract as need testing solution;
4) get the part need testing solution, splash into the trinitrophenol saturated aqueous solution, carry out chemical reaction I;
5) get the part need testing solution in addition, splash into test solution of mercuric potassium iodide, carry out chemical reaction II;
6) judgement of testing result: chemical reaction I and II all produce precipitation or muddy, then are judged as and contain gliclazide in the testing sample.
Before the resulting treated testing sample of step 1) extracts with organic solvent, splash into small amount of alkali solution earlier.
Organic solvent of the present invention is for dissolving each other mutually with water and to the organic solvent that gliclazide has good solubility, comprising methenyl choloride, methylene chloride, cyclohexane etc., wherein methenyl choloride preferably.
Aqueous slkali of the present invention is selected from NaOH solution or KOH solution.The concentration of described aqueous slkali is 0.14mol/L～0.18mol/L, wherein 0.15mol/L preferably.
The processing of the described testing sample of step 1) comprises following method:
Tablet: crushing, get powder;
Pill: smash to pieces, get powder;
Capsule: directly get content;
Granule: porphyrize, get powder.
Step 2) resulting extract is adding before aqueous slkali extracts, and is that the organic system miillpore filter of 0.45 μ m filters with the aperture earlier.When the adding aqueous slkali extracted in step 3), aqueous slkali was 1: 1 with the volume of organic solvent ratio.
The resulting need testing solution of step 3) is that the organic system miillpore filter of 0.45 μ m filters with the aperture earlier before carrying out the described chemical reaction of step 4) and step 5).
In step 4), the volume ratio of need testing solution and trinitrophenol saturated aqueous solution is 1: 1.25～1: 3, wherein preferably 1: 2～1: 3.In step 5), the volume ratio of need testing solution and test solution of mercuric potassium iodide is 1: 0.3～1: 1, wherein preferably 1: 0.6.
Because contain a large amount of pigments in the Chinese patent drug, it is water-soluble or pure molten that its composition mostly is, water is carried, alcohol extracting all has pigment to disturb, and the preferred methenyl choloride of the present invention extracts, and can extract gliclazide effectively, can remove the interference of a large amount of pigments again.In addition, because most hypoglycemic pcms all contain viscosity compositions such as glutinous rehmannia, directly extract with methenyl choloride, extract is difficult to separate with medicinal powder, can make extract be easy to separate with medicinal powder but splash into small amount of alkali solution.
Sulfonylurea hypoglycemic Western medicine, as gliclazide, glibenclamide, gliquidone, Glipizide, Glimepiride, orinase etc., owing to contain the structure of urea in the molecule, can react with trinitrophenol, form yellow muddy or precipitation, and other non-sulfonylurea hypoglycemic Western medicine, example hydrochloric acid melbine, DB2, PIOGITAZONE HYDROCHLORIDE, Luogelie ketone hydrochloride, Repaglinide, Rosiglitazone, Rosiglitazone Maleate etc. can not form muddiness or precipitation with the trinitrophenol reagent reacting.Therefore, when the described chemical reaction I of step 4) produces yellow mercury oxide or muddiness, can judge and contain sulfonylurea hypoglycemic Western medicine in the testing sample.Moreover, because gliclazide is for containing the N heterogeneous ring compound, can react with potassium mercuric iodide, produce white casse or precipitation, and other common sulfonylurea hypoglycemic Western medicine, as glibenclamide, gliquidone, Glipizide, Glimepiride, orinase etc., all can not form muddy or precipitation with the potassium mercuric iodide reaction.Therefore, when the described chemical reaction II of step 5) produces white precipitate or muddiness, can further judge and contain gliclazide in the testing sample.
Illegal detection method of adding gliclazide can extract gliclazide effectively in the hypoglycemic pcm of the present invention, can remove the interference of a large amount of pigments again; Both formed coloured precipitation reaction, can finish at short notice again, met the requirement of " examining method soon ", used when can be used as on-the-spot supervision and check.In addition, the present invention has adopted the chemical reaction of two high specificities as detection means, has sensitivity, advantage such as reliable.
In addition, " discrimination method under second the 595th page " gliclazide " item of Chinese pharmacopoeia version in 2005 is: gliclazide is dissolved in the pyridine, drips CuSO again
4Test solution makes to form complex compound generation bluish violet.But there are two shortcomings in this discrimination method: 1, pyridine has the special gas of smelling, and pollutes lab space and makes the experimenter be difficult to bear; 2, screening property is not strong, glibenclamide, gliquidone, Glipizide, Glimepiride, orinase etc. also can with CuSO
4Test solution produces bluish violet.Detection method of the present invention can be used for the routine of gliclazide equally and differentiate: gliclazide is dissolved in 0.15mol/L NaOH solution, splash into trinitrophenol saturated aqueous solution and test solution of mercuric potassium iodide respectively, both all produce precipitation or muddiness can be differentiated and is gliclazide.This method can overcome the defective of present discrimination method, helps that perfect " Chinese pharmacopoeia is carried the discrimination method of record.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.
Test one:
Taking off and stating sample number into spectrum in the table 1 is each a slice of hypoglycemic Western medicine of 1～12, puts respectively in the 10ml scale test tube after being pressed into powder, and each adds the NaOH solution of 2ml 0.15mol/L.Jolting or sonicated 10 minutes left standstill 5 minutes then, can carry out centrifugal in case of necessity.Draw supernatant with syringe respectively, the organic system miillpore filter with 0.45 μ m filters then.Respectively get 0.8ml filtrate, splash into 1ml trinitrophenol saturated aqueous solution respectively, carry out chemical reaction I.
Test findings shows: sample number into spectrum is that 1～6 medicine all produces tangible yellow mercury oxide in the table 1, and sample number into spectrum is that 7～12 medicine does not all produce any precipitation.This is because sample number into spectrum is that 1～6 medicine belongs to sulfonylureas in the table 2, can form yellow mercury oxide with the trinitrophenol reaction, and sample number into spectrum to be 7～12 medicine all do not belong to sulfonylureas, so can not produce any precipitation.
Get 0.15mol/L NaOH solution 2ml, put in the test tube, splash into 1ml trinitrophenol saturated aqueous solution then, do not produce any precipitation, illustrate that reagent itself is noiseless to testing.
Test two:
Taking off and stating sample number into spectrum in the table 1 is each a slice of hypoglycemic Western medicine of 1～6, puts respectively in the 10ml scale test tube after being pressed into powder, and each adds the NaOH solution of 2ml 0.15mol/L.Jolting or sonicated 10 minutes left standstill 5 minutes then, can carry out centrifugal in case of necessity.Draw supernatant with syringe respectively, the organic system miillpore filter with 0.45 μ m filters then.Respectively get 0.8ml filtrate, splash into the 0.4ml test solution of mercuric potassium iodide respectively, carry out chemical reaction II.
Test findings shows: sample number into spectrum is that 1 medicine (gliclazide sheet) produces tangible white precipitate in the table 1, and sample number into spectrum is that 2～6 medicine does not all produce any precipitation.This is because gliclazide is to contain the N heterogeneous ring compound, can form white precipitate with the potassium mercuric iodide reaction.
Get 0.15mol/L NaOH solution 2ml, put in the test tube, splash into the 0.4ml test solution of mercuric potassium iodide then, do not produce any precipitation, illustrate that reagent itself is noiseless to testing.
Table 1 hypoglycemic Western medicine sample
| Sample number into spectrum | The sample title | Factory's name | Specification | Lot number |
| 1 | The gliclazide sheet | The Beijing JingFeng Pharmaceutical Co., Ltd | 0.4g/ sheet | 20070702 |
| 2 | The glibenclamide sheet | Guangdong three is medical Group Co.,Ltd | 0.3g/ sheet | 20070801 |
| 3 | The gliquidone sheet | The Beijing WanHui ShuangHe pharmacy Co.,Ltd | 0.3g/ sheet | 20080701 |
| 4 | Glipizide tablet | Hainan Zan Bang pharmaceutical Co. Ltd | 0.25g/ sheet | L00208 |
| 5 | Glimepiride tablet | Guizhou Shengjitang Pharmaceutical Co., Ltd. | 0.42g/ sheet | 20080801 |
| 6 | Orinase | Guangzhou Central Ye Pharmaceutical Co., Ltd | Raw material | -------- |
| 7 | Metformin hydrochloride tablet | Shenzhen China Associated Pharmaceutical Co., Ltd. | The 12g/ bag | 70915 |
| 8 | Phenformin hydrochloride tablet | Jiangsu Yabang Aipusen Pharmaceutical Co., Ltd. | 0.3g/ sheet | 20080301 |
| 9 | The PIOGITAZONE HYDROCHLORIDE sheet | Chongqing Kerui Pharmaceutical Co | The 9g/ bag | 20080409 |
| 10 | The Repaglinide sheet | Denmark Novo Nordisk Co.,Ltd | The 3g/ bag | 711529 |
| 11 | The Rosiglitazone sheet | Chengdu Hengrui Pharmaceutical Co., Ltd | -------- | 20080416 |
| 12 | The Rosiglitazone Maleate sheet | GlaxoSmithKline PLC (Tianjin) company limited | 0.5g/ sheet | 2008070129 |
Test three:
Taking off respectively and stating sample number into spectrum in the table 2 is 1～16 hypoglycemic pcm, handles by the following method:
Tablet: (0.3g～0.5g), remove dressing crushes, and gets powder to get 1;
Pill: get 0.5g, smash to pieces, get powder;
Capsule: (0.3g～0.5g), remove softgel shell directly gets content to get 1;
Granule: get 0.5g, porphyrize is got powder;
Treated testing sample is placed 10ml tool plug scale test tube respectively, respectively splash into the NaOH solution of 1 0.15mol/L, add the 6ml methenyl choloride again.The stoppered test tube plug, firmly jolting or sonicated are 10 minutes, leave standstill then 3～5 minutes.Draw the 4ml extract with syringe respectively, behind the organic system filtering with microporous membrane of 0.45 μ m, place another 10ml tool plug scale test tube respectively, each adds the NaOH solution of 4ml 0.15mol/L, and jolting 3～5 times was left standstill 5 minutes.Draw the NaOH solution layer extract on upper strata respectively with syringe, the organic system miillpore filter with 0.45 μ m filters then, and gained filtrate is as need testing solution.
Get above-mentioned need testing solution 1.6ml respectively, average mark places two test tubes, every test tube 0.8ml.Splash into 1.5ml～2ml trinitrophenol saturated aqueous solution in a test tube therein, carry out chemical reaction I.If do not produce muddy or precipitation, but then do not contain sulfonylurea hypoglycemic Western medicine in the judgement sample; If produce significantly yellow muddy or precipitation, but then contain sulfonylurea hypoglycemic Western medicine in the judgement sample.
In another test tube, splash into the 0.5ml test solution of mercuric potassium iodide, carry out chemical reaction II, can not the jolting test tube after splashing into process and dripping off.If do not produce muddy or precipitation, but then do not contain gliclazide in the judgement sample; If produce tangible white opacity or precipitation, but then contain gliclazide in the judgement sample.
Test findings shows: sample number into spectrum is that 1～16 medicine does not all produce any precipitation in chemical reaction I and II in the table 2, illustrates that negative reaction all is negative, no false negative.
Test four:
Taking off respectively and stating sample number into spectrum in the table 2 is 1～16 hypoglycemic pcm, (Beijing JingFeng Pharmaceutical Co., Ltd produces the gliclazide sheet of the artificial 40mg of interpolation, rules are the 80mg/ sheet, and lot number is 080302), according to test three described methods sample is handled then.
Treated testing sample is placed 10ml tool plug scale test tube respectively, respectively splash into the NaOH solution of 1 0.15mol/L, add the 6ml methenyl choloride again.The stoppered test tube plug, firmly jolting or sonicated are 10 minutes, leave standstill then 3～5 minutes.Draw the 4ml extract with syringe respectively, behind the organic system filtering with microporous membrane of 0.45 μ m, place another 10ml tool plug scale test tube respectively, each adds the NaOH solution of 4ml 0.15mol/L, and jolting 3～5 times was left standstill 5 minutes.Draw the NaOH solution layer extract on upper strata respectively with syringe, the organic system miillpore filter with 0.45 μ m filters then, and gained filtrate is as need testing solution.
Get above-mentioned need testing solution 1.6ml respectively, average mark places two test tubes, every test tube 0.8ml.Splash into 1.5ml～2ml trinitrophenol saturated aqueous solution in a test tube therein, carry out chemical reaction I.If do not produce muddy or precipitation, but then do not contain sulfonylurea hypoglycemic Western medicine in the judgement sample; If produce significantly yellow muddy or precipitation, but then contain sulfonylurea hypoglycemic Western medicine in the judgement sample.
In another test tube, splash into the 0.5ml test solution of mercuric potassium iodide, carry out chemical reaction II, can not the jolting test tube after splashing into process and dripping off.If do not produce muddy or precipitation, but then do not contain gliclazide in the judgement sample; If produce tangible white opacity or precipitation, but then contain gliclazide in the judgement sample.
Test findings shows: sample number into spectrum is that 1～16 medicine all produces tangible yellow mercury oxide in chemical reaction I in the table 2, and all produces tangible white precipitate in chemical reaction II, illustrates that positive reaction all is positive, non-false positive.
Table 2 hypoglycemic pcm sample
| Sample number into spectrum | The sample title | Factory's name | Specification | Lot number |
| 1 | Ten Six-element wasting-thirst capsules | The important company limited in the Yellow River, Shandong | 0.4g/ grain | 20070702 |
| 2 | The happy capsule of sugar urea | Guangdong Shen Wei pharmaceutcal corporation, Ltd | 0.3g/ grain | 20070801 |
| 3 | Capsule for lowering blood sugar and preventing thirst | Shandong side is good for pharmaceutical Co. Ltd | 0.3g/ grain | 20080701 |
| 4 | Diabetes pill | Guangzhou Zhongyi Medicine Industry Co., Ltd | 0.25g/ grain | L00208 |
| 5 | Blood-sugar reducing tablets | Heilongjiang Tianhong Pharmaceutical Co., Ltd. | 0.42g/ sheet | 20080801 |
| 6 | The clever sheet of quenching one's thirst | Siping City Ji Te pharmaceutcal corporation, Ltd | 0.36g/ sheet | 20080201 |
| 7 | The ginseng, astragalus diabetes particle | Xi'an miracle pharmaceutical Co. Ltd | The 12g/ bag | 70915 |
| 8 | The happy capsule of sugar urea | Guangdong Shen Wei pharmaceutcal corporation, Ltd | 0.3g/ grain | 20080301 |
| 9 | The recovering particles of quenching one's thirst | Shannxi Aimin Pharmaceutical Co., Ltd. | The 9g/ bag | 20080409 |
| 10 | SHENQI JIANGTANG KELI | Lunan Pharmaceutical Co., Ltd. | The 3g/ bag | 711529 |
| 11 | Melbine | Yangjiang City institute of traditional Chinese medicine | 60 slices/bottle | 20080416 |
| 12 | The hall capsule of meals | The hall diabetes of Shenzhen meals eat product scientific and technological development company limited | 0.5g/ grain | 2008070129 |
| 13 | SHENSHI JIANGTANG JIAONANG | Henan Lingrui Pharmacy Stock Co., Ltd | 0.35g/ grain | 080613 |
| 14 | Gold stilbene Jiangtang capsule | Jilin Aodong Yanbian Medicine Industry Co., Ltd | 0.4g/ grain | 0711001 |
| 15 | The clever sheet of quenching one's thirst | Changchun Yin Nuoke pharmaceutcal corporation, Ltd | 0.36g/ sheet | 20070502 |
| 16 | The hypoglycemic Yiganning capsule | Henan Purentang Pharmacy Co.,Ltd | 0.4g/ grain | 20090301 |
The statistics of test findings:
Test findings to above-mentioned test one to four is added up, and is as follows:
Table 3 true positives, false positive, true negative and false negative statistics
Sensitivity (Se): Se=A/ (A+C) * 100%=16 ÷ 16 * 100%=100%
Specificity (Sp): Sp=D/ (B+D) * 100%=16 ÷ 16 * 100%=100%
Loss (OT): OT=C/ (A+C) * 100%=0 ÷ 16 * 100%=0
False drop rate (MT): MT=B/ (B+D) * 100%=0 ÷ 16 * 100%=0
Accuracy (AR): AR=(A+D)/(A+B+C+D) * 100%
＝32÷32×100％
＝100％
Correct index (AI): AI=1-MT-OT=1-0-0=1
Lowest detectable limit: get the arbitrary sample in the table 2, add the gliclazide (plain sheet) of 2mg, 4mg, 6mg, 8mg and 10mg respectively, test according to test four described methods.The result shows: when the addition of gliclazide was 6mg, chemical reaction I and chemical reaction II can just produce muddiness.Therefore, the lowest detection of detection method of the present invention is limited to: every milliliter aqueous slkali contains the 0.80mg gliclazide.
Claims (10)
1, illegal detection method of adding gliclazide in a kind of hypoglycemic pcm may further comprise the steps:
1) processing of testing sample;
2) treated testing sample extracts with organic solvent, obtains the extract of testing sample;
3) add aqueous slkali in the resulting extract and extract, get aqueous slkali layer extract as need testing solution;
4) get the part need testing solution, splash into the trinitrophenol saturated aqueous solution, carry out chemical reaction I;
5) get the part need testing solution in addition, splash into test solution of mercuric potassium iodide, carry out chemical reaction II;
6) judgement of testing result: chemical reaction I and II all produce precipitation or muddy, then are judged as and contain gliclazide in the testing sample.
2, detection method according to claim 1 is characterized in that: before the resulting treated testing sample of step 1) extracts with organic solvent, splash into aqueous slkali earlier.
3, detection method according to claim 1 and 2 is characterized in that: described organic solvent is the organic solvent that does not dissolve each other mutually and gliclazide is had good solubility with water.
4, detection method according to claim 3 is characterized in that: described organic solvent is selected from methenyl choloride, methylene chloride or cyclohexane.
5, detection method according to claim 1 and 2 is characterized in that: described aqueous slkali is selected from NaOH solution or KOH solution.
6, detection method according to claim 5 is characterized in that: the concentration of described aqueous slkali is 0.14mol/L～0.18mol/L.
7, detection method according to claim 1 and 2 is characterized in that: step 2) resulting extract adding before aqueous slkali extracts, and is that the organic system miillpore filter of 0.45 μ m filters with the aperture earlier; When the adding aqueous slkali extracted in step 3), aqueous slkali was 1: 1 with the volume of organic solvent ratio.
8, detection method according to claim 1 and 2 is characterized in that: the resulting need testing solution of step 3) is that the organic system miillpore filter of 0.45 μ m filters with the aperture earlier before carrying out the described chemical reaction of step 4) and step 5).
9, detection method according to claim 1 and 2 is characterized in that: in step 4), the volume ratio of need testing solution and trinitrophenol saturated aqueous solution is 1: 1.25～1: 3.
10, detection method according to claim 1 and 2 is characterized in that: in step 5), the volume ratio of need testing solution and test solution of mercuric potassium iodide is 1: 0.3～1: 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2009100401256A CN101581710A (en) | 2009-06-10 | 2009-06-10 | Method for detecting illegally added gliclazide in hypoglycemic Chinese patent medicament |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2009100401256A CN101581710A (en) | 2009-06-10 | 2009-06-10 | Method for detecting illegally added gliclazide in hypoglycemic Chinese patent medicament |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101581710A true CN101581710A (en) | 2009-11-18 |
Family
ID=41363950
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2009100401256A Pending CN101581710A (en) | 2009-06-10 | 2009-06-10 | Method for detecting illegally added gliclazide in hypoglycemic Chinese patent medicament |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101581710A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103645179A (en) * | 2013-11-11 | 2014-03-19 | 江苏省食品药品检验所 | Method for rapidly detecting sulfonylomocznik compound added in hypoglycemic health foods, Chinese patent medicines and foodstuff and applications thereof |
| CN106596545A (en) * | 2016-12-12 | 2017-04-26 | 广州安诺食品科学技术有限公司 | Rapid detection method of sulfonylurea chemical constituents |
| CN111426683A (en) * | 2020-06-10 | 2020-07-17 | 广州智汇生物科技有限公司 | Method for detecting sulfonylureas drug components in hypoglycemic health products |
-
2009
- 2009-06-10 CN CNA2009100401256A patent/CN101581710A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103645179A (en) * | 2013-11-11 | 2014-03-19 | 江苏省食品药品检验所 | Method for rapidly detecting sulfonylomocznik compound added in hypoglycemic health foods, Chinese patent medicines and foodstuff and applications thereof |
| CN106596545A (en) * | 2016-12-12 | 2017-04-26 | 广州安诺食品科学技术有限公司 | Rapid detection method of sulfonylurea chemical constituents |
| CN111426683A (en) * | 2020-06-10 | 2020-07-17 | 广州智汇生物科技有限公司 | Method for detecting sulfonylureas drug components in hypoglycemic health products |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101581712B (en) | Quick test method of biguanide compounds added in hypoglycemic medicine, health care products or food and application thereof | |
| CN101581710A (en) | Method for detecting illegally added gliclazide in hypoglycemic Chinese patent medicament | |
| CN110143920A (en) | The extraction preparation method of Sinomenine in a kind of caulis sinomenii | |
| CN101822765A (en) | Quality inspection method of traditional Chinese medicine compound preparation with functions of tonifying kidney, strengthening bones, enriching blood and being beneficial to sperm | |
| CN108693265A (en) | The extraction and purifying of HERBA DENDROBII total alkaloid and content assaying method | |
| CN108250320A (en) | A kind of low ash content ganoderan extract and preparation method thereof | |
| CN102353747B (en) | Detection method of rosiglitazone or pioglitazone in Chinese patent medicine and health food | |
| CN101672792A (en) | Detection method of quinolone drugs, detection reagent kit and application | |
| CN113759065B (en) | Method for simultaneously identifying components of coptis chinensis and phellodendron amurense and application of method | |
| CN101408519B (en) | Method for detecting sibutramine hydrochloride and application thereof | |
| CN103645179A (en) | Method for rapidly detecting sulfonylomocznik compound added in hypoglycemic health foods, Chinese patent medicines and foodstuff and applications thereof | |
| CN101692079A (en) | Rapid detection method and rapid detection kit of fluoroquinolone antibiotics | |
| CN101269097A (en) | Alstonia-leaf medicinal materials and medicament testing method for its preparation | |
| CN105866232B (en) | The method for measuring total amount mercury and valence state mercury content in living organism tissue and internal organs | |
| CN104076036B (en) | The method of biguanides in detection goods | |
| CN102125622A (en) | Detection method of traditional Chinese medicine preparation for clearing away heat and toxic material, removing food retention and regulating stomach | |
| CN110967430B (en) | Method for measuring dissolution curve of coenzyme Q10 capsule | |
| CN103499653B (en) | The fingerprint atlas detection method of Zhenju Jiangya Tablet and application thereof | |
| CN112730665A (en) | Chromatographic method for measuring vitamin A content by ultra-high performance liquid chromatography | |
| CN102631441B (en) | Separation and purification method of total saponins of sanguisorba officinalis | |
| CN106525842A (en) | Quick detection method of dexamethasone | |
| CN100509018C (en) | Preparation of Japanese beauty-berry and inspection method thereof | |
| CN101598715B (en) | Rapid detection method of lafil PDE5 type inhibitor in drugs, health foods and foods | |
| CN102058829A (en) | Medicine composition and detection method of preparations of medicine composition | |
| Bandelin et al. | Colorimetric determination of thiamine in pharmaceutical products |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C41 | Transfer of patent application or patent right or utility model | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20091030 Address after: 4, south suburb village, Jiangcheng District, Guangdong, Yangjiang Applicant after: Huang Wen Feng Co-applicant after: Lin Ruiqun Co-applicant after: Yao Wuhu Co-applicant after: Feng Gang Address before: Guangdong Province, Yangjiang City, Jiangcheng District, the southern suburbs of the village on the 4th Applicant before: Huang Wenfeng |
|
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| AD01 | Patent right deemed abandoned |
Effective date of abandoning: 20091118 |
|
| C20 | Patent right or utility model deemed to be abandoned or is abandoned |