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Method for determining residue of methaqualone and diazepam in animal-derived food

A determination method and animal-derived technology, which are applied in the field of determination of the residues of meprodone and diazepam in animal-derived foods, can solve the problems of complicated operation, many interferences, low sensitivity of high-performance liquid chromatography, etc., and achieve qualitative and quantitative results. Scientific and accurate, strong anti-interference ability, wide range of effects

Active Publication Date: 2017-06-13
INSPECTION & QUARANTINE TECH CENT OF GUANGDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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Problems solved by technology

However, the former gas chromatography-mass spectrometry method is cumbersome to operate and has more interference, which is not suitable for the rapid analysis of large quantities of samples; the latter high-performance liquid chromatography method has a lower limit of 10 μg / kg, which cannot meet the technical requirements of 1.0 μg issued by the regulatory authorities / kg, high performance liquid chromatography has low sensitivity, large matrix interference, and no application value; the following are the specific comparison results

Method used

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  • Method for determining residue of methaqualone and diazepam in animal-derived food
  • Method for determining residue of methaqualone and diazepam in animal-derived food
  • Method for determining residue of methaqualone and diazepam in animal-derived food

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Embodiment 1

[0095] 1. Principle

[0096] The sample was extracted with ethyl acetate, the extract was purified by QuEChERs (Quick, Easy, Cheap, Effective, Rugged, Safe) purification tube, concentrated and evaporated to dryness, the residue was dissolved in mobile phase, and detected by liquid chromatography-tandem mass spectrometer, the internal Quantification by standard method.

[0097] 2. Reagents and Materials

[0098] The reagents used below are all analytical reagents unless otherwise specified; the water is first-class water in accordance with GB / T 6682.

[0099] 2.1 Standard solution of methadrax: 0.1mg / mL, LGC company.

[0100] 2.2 Diazepam standard solution: 100 μg / mL Cerilliant Company.

[0101] 2.3 Diazepam isotope internal standard standard solution: deuterated diazepam (D 5 - diazepam) 1.0 mg / mL Cerilliant.

[0102] 2.4 Acetonitrile: chromatographically pure, Fisher Company.

[0103] 2.5 Ethyl acetate: Guangzhou Chemical Reagent Factory.

[0104] 2.6 Formic acid: chro...

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Abstract

The invention discloses a method for determining residue of methaqualone and diazepam in animal-derived food like pork, fish, pig liver and pig kidney. The method includes: adopting ethyl acetate as an extraction solvent; purifying through a mixed powder pipe; using a liquid chromatography-tandem mass spectrometer for detection; adopting an internal standard method for quantification. Regression equation correlation coefficient reaches higher than 0.99, determination lower limit is 0.5ug / kg, recycling rate on adding concentration level of 0.5-5ug / kg is 90-120%, and relative standard deviation in a lab is lower than or equal to 15%. The method is simple and convenient to operate, high in sensitivity and interference resistance, wide in matrix adapting range, scientific and accurate in qualification and quantification, suitable for quick analysis of mass samples and capable of meeting technical requirements of related supervision departments of China.

Description

technical field [0001] The invention belongs to the technical field of detection of veterinary drug residues in food, and in particular relates to a method for determining the residual amount of methadrax and diazepam in animal source food. Background technique [0002] Methaquinone and diazepam are clinically used as sedative hypnotics, which belong to psychotropic drugs, and long-term use can cause addiction and dependence. In recent years, with the development of animal husbandry, some criminals, driven by economic interests, have added and used it in livestock and poultry breeding without authorization, in order to increase meat production. In addition, the use during transportation can also play a role in keeping alive and keeping weight. The abuse of methadrax and diazepam will lead to drug residues in animal-derived foods, which will eventually seriously affect the health of consumers. [0003] Announcement No. 235 of the Ministry of Agriculture of my country has cl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/14
CPCG01N30/02G01N30/14
Inventor 邵琳智陈思敏徐娟卢丽邹游蓝草
Owner INSPECTION & QUARANTINE TECH CENT OF GUANGDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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