Liquid chromatography-tandem mass spectrometry method used for simultaneous detection of 10 kinds 94 residual drugs in livestock and poultry

A technology of residual drugs and liquid chromatography, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of simultaneous purification of multiple types of veterinary drugs, and achieve the effect of rapid detection methods, improved efficiency, and economical use

Inactive Publication Date: 2018-06-08
ZHEJIANG INST FOR FOOD & DRUG CONTROL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the solid-phase small column also has relative limitations, and can only be applied to the purification of various veterinary drugs, but cannot realize the simultaneous purification of multiple types of veterinary drugs.

Method used

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  • Liquid chromatography-tandem mass spectrometry method used for simultaneous detection of 10 kinds 94 residual drugs in livestock and poultry
  • Liquid chromatography-tandem mass spectrometry method used for simultaneous detection of 10 kinds 94 residual drugs in livestock and poultry
  • Liquid chromatography-tandem mass spectrometry method used for simultaneous detection of 10 kinds 94 residual drugs in livestock and poultry

Examples

Experimental program
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Effect test

preparation example Construction

[0100] A. Preparation of internal standard stock solution:

[0101] Dilute 1mg of sulfamethazine-d5, sulfamethazine-D5, demetonidazole-D3, hydrocortisone-D3, thiamphenicol-D3, florfenicol-D3, clindamycin respectively with methanol Sodium-D3 and erythromycin-13CD2 were respectively dissolved in 10mL volumetric flasks to prepare an internal standard stock solution with a concentration of 100μg / mL, stored at -18°C in the dark, and valid for 1 year. Nalidixic acid-D5, norfloxacin-D5, pefloxacin-D5, enrofloxacin-D5, flufloxacin-D3, and chloramphenicol-D5 are commercial reference solutions with a concentration of 100 μg / mL .

[0102] B. Preparation of isotope internal standard working mixture: Precisely measure 0.050mL of each of the above-mentioned standard stock solutions in a 20.0mL volumetric flask, dilute with methanol to constant volume, and prepare mixed standard working solutions with concentrations of 250μg / L, respectively, - Store in the dark at 18°C, valid for 2 months....

Embodiment 1

[0119] A liquid chromatography-tandem mass spectrometry method for the simultaneous determination of 94 drug residues in 10 categories in livestock and poultry, including:

[0120] Sample preparation steps: Take the chicken sample, remove the skin and bones, and use a meat grinder to make meat paste for the meat tissue part, obtain the sample to be tested, mix it and put it in a sealed packaging bag, and store it in a freezer below -18°C for later use;

[0121] Extractant preparation steps: take acetonitrile, water and formic acid, mix them evenly, and obtain the extractant; wherein, the volume ratio of water, acetonitrile and formic acid is 20:80:0.1;

[0122] Sample extraction steps: Accurately weigh 2.0 g of the sample to be tested, place it in a 50 mL centrifuge tube, accurately add 0.2 mL of the isotope internal standard working mixture, then add 9.8 mL of the extractant, homogenize at a speed of 12000 r / min for 2 min, Obtain the first analysis solution; centrifuge the fi...

Embodiment 2

[0135] The difference between embodiment 2 and embodiment 1 is: in the extractant, the volume ratio of water and acetonitrile is 10:90. Others are identical with specific embodiment 1.

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Abstract

The invention discloses a liquid chromatography-tandem mass spectrometry method used for simultaneous detection of 10 kinds 94 residual drugs in livestock and poultry. The liquid chromatography-tandemmass spectrometry method used for simultaneous detection of 10 kinds 94 residual drugs in livestock and poultry comprises following steps: sample preparation, wherein livestock and poultry meat is prepared into meat paste so as to obtain samples to be measured; extraction solvent preparation, wherein, acetonitrile, water, and formic acid are mixed to be uniform so as to obtain the extraction solvent; sample extraction, wherein the samples to be measured are weighed, an internal reference working mixed solution is added; homogenizing is carried out after adding of the extraction solvent, centrifugation is carried out, a supernatant liquid 1 is collected; and sample purifying, wherein the solution to be tested is subjected to extraction using an Oasis PriMe HLB solid phase extraction column, the extraction solvent is adopted to washing the solid phase extraction column, and obtained eluants are mixed; nitrogen blowing is carried out, an obtained mixture is diluted to a constant volume,centrifugation is carried out, an obtained supernatant 2 is collected, and filtered so as to obtain a solution to be tested; and measuring, wherein the solution to be tested is subjected to UPLC-MS / MSmeasuring. The liquid chromatography-tandem mass spectrometry method is capable of realizing simultaneous detection of 10 kinds 94 residual drugs in 15min, detection efficiency is increased greatly,labor cost is reduced greatly, the reagents are saved, and the liquid chromatography-tandem mass spectrometry method is green, and is friendly to the environment.

Description

technical field [0001] The invention relates to the technical field of analytical chemistry, in particular to a liquid chromatography-tandem mass spectrometry method for simultaneously determining 94 kinds of residual drugs in 10 categories in livestock and poultry. Background technique [0002] In the process of raising livestock and poultry, most of them use veterinary drugs, so there are generally veterinary drug residues in the bodies of livestock and poultry. Different types of veterinary drugs have different molecular structures, molecular weights, and functional groups, resulting in widely different chemical properties. Therefore, most conventional detection methods can only test one or two types of drugs at the same time. In the livestock and poultry breeding process, multiple types of drugs are often used at the same time, so many different inspection methods are often used in the inspection process, which is time-consuming and laborious, and the workload of the in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/88
CPCG01N30/06G01N30/88
Inventor 陈万勤刘柱沈泓周霞丁宇琦赵超群罗金文陈碧莲
Owner ZHEJIANG INST FOR FOOD & DRUG CONTROL
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