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Detection method of rosiglitazone or pioglitazone in Chinese patent medicine and health food

A detection method and health food technology, applied in the direction of chemical analysis using precipitation, etc., can solve problems such as difficult to make accurate judgments, unclear results, weak chemical alkalinity, etc., to reduce detection costs, easy reaction phenomena, and detection speed fast effect

Active Publication Date: 2012-02-15
广东省药品检验所
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This is mainly due to the following reasons: First, the chemical alkalinity of the doped rosiglitazone and pioglitazone is very weak. If no special extraction and separation steps are taken, although these hypoglycemic compounds can react with the precipitant, they will coexist in the product Other alkaline components in the product will also react, covering up the desired reaction phenomenon, resulting in unclear and unclear results, making it difficult to make accurate judgments
Second, the addition of hypoglycemic ingredients may be a combination of various types. For example, thiazolidinediones may be added in combination with sulfonylureas and biguanides, or sulfonylureas and biguanides may be added separately. It will interfere with the detection and display, and there will be false positives for thiazolidinediones; that is, even if the test is positive, it cannot be judged whether it is rosiglitazone or pioglitazone
However, according to the teaching of this patent technology, in an ethanol environment (as the technical solution of claim 1) or in a non-acidic, non-neutral environment for detection (as described in the penultimate paragraph on page 2 of its specification), the result The error is also extremely obvious (the test result is verified by mass-liquid chromatography technology, and the correct rate is less than 40%)

Method used

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  • Detection method of rosiglitazone or pioglitazone in Chinese patent medicine and health food
  • Detection method of rosiglitazone or pioglitazone in Chinese patent medicine and health food
  • Detection method of rosiglitazone or pioglitazone in Chinese patent medicine and health food

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0117] Test commercially available Tang Niao Le capsules (batch number: 100501): Sinopharm Holding Shenzhen Traditional Chinese Medicine Co., Ltd., 0.3g*30s per bottle. Take orally, 3-4 capsules at a time, 3 times a day.

[0118] Kit composition:

[0119] Reagent 1: dichloromethane (chemically pure);

[0120] Reagent 2: 0.08mol / L hydrochloric acid solution;

[0121] Reagent 3: 0.04 g / mL phosphomolybdic acid solution.

[0122] Take the content of 1 sample to be tested, add 3 mL of dichloromethane and shake vigorously for 40 seconds, then filter; add 2 mL of 0.08 mol / L hydrochloric acid solution to the filtrate, turn it up and down 8 times, and let it stand for 30 seconds to separate the two phases In above-mentioned supernatant liquid, drop into 2 drops concentration and be the phosphomolybdic acid solution of 0.04g / mL.

[0123] Result: No precipitation occurred and the solution was clear.

[0124] Standard method verification: 1 sample to be tested was taken and tested by...

Embodiment 2

[0127] Test commercially available Tang Niao Le capsules (batch number: 100501): Sinopharm Holding Shenzhen Traditional Chinese Medicine Co., Ltd., 0.3g*30s per bottle. Take orally, 3-4 capsules at a time, 3 times a day.

[0128] Kit composition:

[0129] Reagent 1: dichloromethane (chemically pure);

[0130] Reagent 2: 0.1mol / L hydrochloric acid solution;

[0131] Reagent 3: 0.05 g / mL phosphomolybdic acid solution.

[0132] Take the content of 1 sample to be tested, add 3 mL of dichloromethane and shake vigorously for 1 minute, then filter; add 2 mL of 0.1 mol / L hydrochloric acid solution to the filtrate, turn it up and down 10 times, and let it stand for 30 seconds to separate the two phases ; Add 2 drops of phosphomolybdic acid solution with a concentration of 0.05g / mL in the upper layer liquid.

[0133] Result: No precipitation occurred and the solution was clear.

[0134] Standard method verification: 1 sample to be tested was taken and tested by liquid-mass spectrom...

Embodiment 3

[0137] Test commercially available Jiangtangning Capsules (batch number: 1006271): Huizhou Luofushan Pharmaceutical Co., Ltd., 0.4g per capsule, 48 capsules / box. Take orally, 4-6 capsules each time, 3 times a day.

[0138] Kit composition:

[0139] Reagent 1: dichloromethane (analytical pure);

[0140] Reagent 2: 0.12mol / L hydrochloric acid solution;

[0141] Reagent 3: 0.1 g / mL phosphomolybdic acid solution.

[0142] Take the content of 1 sample to be tested, add 2 mL of dichloromethane and shake vigorously for 1 minute, then filter; add 3 mL of 0.12 mol / L hydrochloric acid solution to the filtrate, turn it up and down 10 times, and let it stand for 45 seconds to separate the two phases ; Add 1 drop of phosphomolybdic acid solution with a concentration of 0.1 g / mL in the above supernatant.

[0143] Result: No precipitation occurred and the solution was clear.

[0144] Standard method verification: 1 sample to be tested was taken and tested by liquid-mass spectrometry. Th...

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Abstract

The invention relates to a detection method for qualitatively detecting whether thiazolidinedione medicines are doped in a Chinese patent medicine and a health food which have a hypoglycemic effect. The method comprises the following steps: 1, taking a sample to be measured, adding dichloromethane according to a case that 5-10mL of dichloromethane corresponds with 1g of the sample, strongly shaking for at least 40s, and filtering; 2, adding a small amount of a hydrochloric acid solution with the concentration of 0.08-0.12mol / L to a filtrate obtained in step 1, up-down overturning at least eight times, and standing for two-phase layering; and 3, adding a proper amount of a phosphomolybdic acid solution with the concentration of 0.04-0.1g / mL to an upper layer obtained in step 2 drop by drop. If deposition or turbidity appears, it shows that rosiglitazone or pioglitazone is doped in the sample. A corresponding kit comprises a reagent 1: dichloromethane; a reagent 2: the hydrochloric acid solution with the concentration of 0.08-0.12mol / L; and a reagent 3: the phosphomolybdic acid solution with the concentration of 0.04-0.1g / mL. The detection method of the invention has the advantages of accuracy and reliability, and the kit is convenient for carrying and carrying out onsite detection.

Description

technical field [0001] The present invention relates to a method for qualitatively detecting the presence or absence of chemical substances, in particular to whether Chinese patent medicines and health foods with hypoglycemic effects are doped with thiazolidinediones, mainly rosiglitazone or pioglitazone. Detection method. Background technique [0002] There are many drugs for the treatment of diabetes. In the early 1980s, chlorpropamide and tolbutamide were often used, and later developed into many categories. Existing drugs for the treatment of diabetes can be roughly divided into five categories, namely sulfonylurea drugs, biguanide drugs, α-glucosidase inhibitors, thiazolidinediones (TZD) drugs and non-sulfonylurea insulin secretagogues . The toxic and side effects shown after taking these chemical drugs reach a certain amount are just very obvious, as: oral hypoglycemic drug rosiglitazone or pioglitazone (especially overdose) may have the risk of raising the patient's...

Claims

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Application Information

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IPC IPC(8): G01N31/02
Inventor 肖树雄李杨杰
Owner 广东省药品检验所
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