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Method for rapidly detecting sulfonylomocznik compound added in hypoglycemic health foods, Chinese patent medicines and foodstuff and applications thereof

A technology of health food and detection method, which is applied in the direction of analyzing materials through chemical reactions and observing the influence of chemical indicators. Detection and other problems, to achieve the effect of strong anti-interference ability of coexisting substances, high accuracy of test conclusions, and easy judgment of color rendering results

Inactive Publication Date: 2014-03-19
江苏省食品药品检验所 +2
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The advantage of thin-layer chromatography is that it does not need to use expensive analytical instruments, but this method is greatly affected by external conditions, the ratio shift value is unstable, there are edge effects, and the chromatographic development and drying time are long, which cannot meet the requirements of rapid determination. Requirements, and high requirements for instruments and the surrounding environment, but also high technical requirements for experimenters
The advantages of high performance liquid chromatography are high chromatographic separation efficiency and high sensitivity, but its disadvantages are that the instrument is expensive, the sample pretreatment time is long, the chromatographic column is easily polluted, the analysis cost is high, the instrument has high requirements for the use environment, and a fixed pendulum is required. High performance liquid chromatography-mass spectrometry is suitable for the analysis of samples with complex components and severe background interference. This analysis method can improve the reliability of the test results, but the method is more complicated to operate , the instrument has higher requirements for the use environment
Need fixed placement, not suitable for on-site inspection with high mobility

Method used

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  • Method for rapidly detecting sulfonylomocznik compound added in hypoglycemic health foods, Chinese patent medicines and foodstuff and applications thereof
  • Method for rapidly detecting sulfonylomocznik compound added in hypoglycemic health foods, Chinese patent medicines and foodstuff and applications thereof
  • Method for rapidly detecting sulfonylomocznik compound added in hypoglycemic health foods, Chinese patent medicines and foodstuff and applications thereof

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Experimental program
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Effect test

Embodiment 1

[0040] The detection of embodiment 1 capsule

[0041] Sample: Shuangbao Qingtang, batch number 20120905, capsules, pioglitazone and glibenclamide were detected by HPLC-MS.

[0042] Adopt rapid detection method of the present invention to measure sample, its concrete steps are as follows:

[0043] (1) Take 2 samples, put the contents in a 5ml syringe, add 3ml of dichloromethane, shake for 2 minutes, filter with an organic microporous filter head (0.45um pore size, 12mm outer diameter), and take about 2ml of the filtrate.

[0044] (2) Add 2ml of the above filtrate to a test tube containing about 20mg of vanillin, add 2ml of concentrated sulfuric acid, shake well, put it in a water bath at 80-90°C and heat it for about 1min, until the methylene chloride is basically evaporated, and the color of the solution changes from yellow to Red-brown.

[0045] (3) Let the above solution cool to room temperature, carefully add 5ml of 95% ethanol along the wall, and find that purple appears...

Embodiment 2

[0046] The detection of embodiment 2 capsules

[0047] Sample: Jiuwei Caotang Tiansang Capsules, batch number 130106, capsules, pioglitazone and glibenclamide were detected by HPLC-MS.

[0048] Adopt rapid detection method of the present invention to measure sample, its concrete steps are as follows:

[0049] (1) Take 2 samples, put the contents in a 5ml syringe, add 3ml of dichloromethane, shake for 2 minutes, filter with an organic microporous filter head (0.45um pore size, 12mm outer diameter), and take about 2ml of the filtrate.

[0050] (2) Add 2ml of the above filtrate to a test tube containing about 20mg of vanillin, add 2ml of concentrated sulfuric acid, shake well, put it in a water bath at 80-90°C and heat it for about 1min, until the methylene chloride is basically evaporated, and the color of the solution changes from yellow to Red-brown.

[0051] (3) Let the above solution cool to room temperature, carefully add 5ml of 95% ethanol along the wall, and find that p...

Embodiment 3

[0052] The detection of embodiment 3 capsules

[0053] Sample: Shanqiginseng special capsules, batch number 20110902, capsules, no sulfonylurea hypoglycemic drugs were detected by HPLC-MS.

[0054] Adopt rapid detection method of the present invention to measure sample, its concrete steps are as follows:

[0055] (1) Take 2 samples, put the contents in a 5ml syringe, add 3ml of dichloromethane, shake for 2 minutes, filter with an organic microporous filter head (0.45um pore size, 12mm outer diameter), and take about 2ml of the filtrate.

[0056] (2) Add 2ml of the above filtrate to a test tube containing about 20mg of vanillin, add 2ml of concentrated sulfuric acid, shake well, put it in a water bath at 80-90°C and heat it for about 1min, until the methylene chloride is basically evaporated, and the color of the solution changes from yellow to Red-brown.

[0057] (3) Allow the above solution to cool to room temperature, carefully add 5ml of 95% ethanol along the wall, and fi...

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Abstract

The invention provides a Method for rapidly detecting a sulfonylomocznik compound added in hypoglycemic medicines, health products and foodstuff and applications thereof. The method comprises selecting a tested sample of once taking amount, adding 3ml dichloromethane, shaking out to dissolve, stewing for a moment, and filtrating; selecting 2ml of filtrate, adding 10mg or 20mg of vanillin solid , then adding 2ml of concentrated sulfuric acid solution, heating for 1min in a micro boiling water bath until an upper dichloromethane layer is completely volatilized; and cooling the solution to room temperature, slowly adding 5ml of ethanol, immediately observing color change of a liquid separation layer and an upper layer solution, slightly shaking up if the liquid separating layer changes purple, and determining that sulfonylomocznik compound is added when the liquid separation layer and the upper layer solution change blue. The method and a used kit have advantages of low analysis cost, strong anti-interference capability, no need of special equipment, high sensitivity, obvious easy observation and judgement of chromogenic result, and high correct rate of examination conclusion, and are suitable for on-site rapid detection.

Description

technical field [0001] The present invention relates to the field of drug detection, in particular to the field of detection of illegally added chemicals in hypoglycemic health food, Chinese patent medicine and food, and in particular to a rapid method for adding sulfonylurea compounds to hypoglycemic health food, Chinese patent medicine and food Detection methods and their applications. Background technique [0002] In recent years, with the change of people's eating habits, the incidence of diabetes has been increasing year by year. The clinical demand for hypoglycemic drugs has always been great, especially health food and traditional Chinese medicine hypoglycemic preparations have been paid attention to and widely used in clinic because of their dual effects of treatment and conditioning. But at present, some lawbreakers are arbitrarily mixing chemical hypoglycemic drug ingredients into health food and traditional Chinese medicine hypoglycemic preparations in order to i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/78
Inventor 芦丽宫旭冯有龙曹玲孙晶张再平尚姝吴莉
Owner 江苏省食品药品检验所
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