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Detection method for illegally added medicine in blood fat reducing Chinese patent medicine and health food

A health food and illegally added technology, applied in the field of ultra-high performance liquid chromatography-tandem mass spectrometry, can solve the problems of weak qualitative ability, few detection components, long detection time, etc., and achieve the effect of accurate method, strong specificity and high sensitivity

Inactive Publication Date: 2018-06-15
KUNMING UNIV OF SCI & TECH
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  • Application Information

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Problems solved by technology

The detection methods that have been reported include thin layer chromatography and high performance liquid chromatography, but there are problems of poor selectivity, weak qualitative ability and low sensitivity; there is also liquid chromatography-mass spectrometry, but the detection components are less and the detection time is longer
[0004] The State Food and Drug Administration promulgated the "Detection Method for Illegally Added Drugs in Auxiliary Blood Lipid-Lowering Health Foods" in 2010, but the method only contains 3 kinds of drug ingredients, and the detection time is very long (nearly 40min), and the sensitivity is low

Method used

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  • Detection method for illegally added medicine in blood fat reducing Chinese patent medicine and health food
  • Detection method for illegally added medicine in blood fat reducing Chinese patent medicine and health food
  • Detection method for illegally added medicine in blood fat reducing Chinese patent medicine and health food

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Experimental program
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Effect test

Embodiment 1

[0019] Embodiment 1: investigation verification of experimental method

[0020] (1) Chromatography-mass spectrometry conditions: Chromatographic column: Waters Acquity BEH-C 18 (2.1mm×50mm, 1.7µm);

[0021] Mobile phase: aqueous solution containing 0.05% formic acid (A) - acetonitrile (B) Gradient elution: 0~2.5min, 50%B, 2.5~3.0min, 60%B, 3.0~3.5min, 100%B, 3.5~ 4.0min, 50%B, flow rate 0.15mL / min; column temperature: 25℃; injection volume 5µL. Mass spectrometry conditions: electrospray ion source ESI positive ion mode scan; capillary voltage 2.5kV; desolvation gas temperature 450°C; desolvation gas flow rate 750L / h; cone gas flow rate 45L / h; collision gas is argon; product ion scan and MRM mode simultaneous monitoring;

[0022] Mobile phase: aqueous solution containing 0.75% formic acid (A) - acetonitrile (B) Gradient elution: 0~2.5min, 50%B, 2.5~3.0min, 60%B, 3.0~3.5min, 100%B, 3.5~ 4.0min, 50%B, flow rate 0.25mL / min; column temperature: 35℃; injection volume 0.5µL. ...

Embodiment 2

[0035] Embodiment 2: the mensuration of sample

[0036] (1) Preparation of reference solution

[0037] Lovastatin (batch number: LK10O58, content 98.0%, China Institute for Food and Drug Control), mevastatin (batch number: 2-NYL-167-1, content 98.0%, China Institute for Food and Drug Control), and Simvastatin (batch number: 11-SCC-167-1, content 98.0%, China Institute for Food and Drug Control), pravastatin sodium (batch number: 8-XJZ-27-1, content 98.0%, China Food and Drug Control Research Institute) Institute), fluvastatin sodium (batch number: 7-ABY-122-1, content 98.0%, China Institute for Food and Drug Control), niacin (batch number: LF80N66, content 99.5%, China Institute for Food and Drug Control) 1- 5mg, put in a 10mL volumetric flask, add methanol to dissolve and dilute to the volume, shake well, and use it as the standard stock solution of each standard. According to the mass spectrometry response results of the preliminary analysis, an appropriate amount of the s...

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PUM

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Abstract

The invention discloses a rapid detection method for six blood fat reducing medicine illegally added into Chinese patent medicine and health food with a blood fat reducing function. The rapid detection method comprises the following steps: after carrying out extraction treatment on a sample with methyl alcohol, adopting an ultra-high performance liquid chromatography-tandem mass spectrometry, carrying out chromatographic column separation, using a formic acid solution and acetonitrile as a moving phase for gradient elution, carrying out mass spectrum ESI positive ion and multi-reaction monitoring mode measurement, and carrying out external standard method quantification. The method is good in linear relation, quick, simple, convenient and accurate, can serve as a qualitative and quantitative detection method for illegally added chemical medicine in the blood fat reducing health food, and can be used for screening illegally added chemical medicine in the Chinese patent medicine and health food. Effective basis is provided for controlling the quality of health food and striking the behaviors of illegal addition in health food industry.

Description

technical field [0001] The present invention relates to the field of food and drug safety, in particular to the field of food and drug safety detection, in particular to an ultra-high performance liquid chromatographic method for simultaneously and quickly detecting the illegal addition of 6 kinds of blood lipid-lowering chemical drugs in Chinese patent medicines with blood lipid-lowering effects and health foods- Tandem mass spectrometry method. Background technique [0002] In recent years, the quality of life of our people has improved significantly, and people are paying more and more attention to their own health. They have begun to pay attention to "prevention of diseases" and "health care", which has led to a rapid increase in the interest space of the health care product market, and countless businesses are competing for gold. . However, following food and drug safety problems are increasing, some criminals illegally add chemical drugs to Chinese patent medicines an...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/047G01N2030/062
Inventor 李晓蕾刘春侠杨俊王齐周荣锋贺与平袁锐波
Owner KUNMING UNIV OF SCI & TECH
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