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Method for determining multiresidue of veterinary drugs in animal-derived foods

A technology of animal origin and determination method, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of single testing items, and achieve the effect of less solvent consumption, improved testing efficiency, and avoidance of losses

Active Publication Date: 2014-06-25
烟台杰科检测服务有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The standards in our country are relatively comprehensive, but each standard targets a single test item, such as GB / T20759-2006 "Determination of Sixteen Sulfonamide Residues in Livestock and Poultry Meat by Liquid Chromatography-Tandem Mass Spectrometry", GB / T20366-2006 "Determination of quinolone residues in animal products by liquid chromatography-tandem mass spectrometry", GB / T20756-2006 "Chloramphenicol, thiamphenicol and fluoxetine in edible animal muscle, liver and aquatic products Determination of Phenicol Residues by Liquid Chromatography-Tandem Mass Spectrometry, etc. Therefore, establishing a rapid, effective, sensitive, reliable and practical method for the analysis of veterinary drug residues has important practical significance for food safety

Method used

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  • Method for determining multiresidue of veterinary drugs in animal-derived foods
  • Method for determining multiresidue of veterinary drugs in animal-derived foods
  • Method for determining multiresidue of veterinary drugs in animal-derived foods

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Take the above-mentioned pig lean meat, and detect its veterinary drug residue content, the steps are as follows:

[0032] (1) Extraction: Weigh 3.0 g of uniformly prepared sample into a 50 mL centrifuge tube, add 15 mL of 1% acetic acid acetonitrile solution, vibrate vigorously for 1 min, ultrasonically extract for 20 min, and centrifuge at 4000 r / min for 5 min;

[0033] (2) Purification: transfer all the acetonitrile extracts obtained after centrifugation in step (1) to a mixed filler (10g anhydrous sodium sulfate, 500mgC 18 and 200mgPSA), vortexed for 1min, centrifuged at 4000r / min for 5min, accurately pipette 5.0mL supernatant to 10mL graduated test tubes I and II with stoppers, and concentrated to near dryness by nitrogen blowing in a water bath at 45°C , add 0.5mL of a mixture of 0.1% formic acid acetonitrile and water with a volume ratio of 2:3 to test tube I to make up to volume, add 0.5mL acetonitrile to test tube to make up to volume, ultrasonicate for 30s, vo...

Embodiment 2

[0051] Take the above-mentioned chicken, and detect its veterinary drug residue content, the steps are as follows:

[0052](1) Extraction: Weigh 3.0 g of uniformly prepared sample into a 50 mL centrifuge tube, add 15 mL of 1% acetic acid acetonitrile solution, vibrate vigorously for 1 min, ultrasonically extract for 20 min, and centrifuge at 4000 r / min for 5 min;

[0053] (2) Purification: transfer all the acetonitrile extracts obtained after centrifugation in step (1) to a mixed filler (10g anhydrous sodium sulfate, 500mgC 18 and 200mgPSA), vortexed for 1min, centrifuged at 4000r / min for 5min, accurately pipette 5.0mL supernatant to 10mL graduated test tubes I and II with stoppers, and concentrated to near dryness by nitrogen blowing in a water bath at 45°C , add 0.5mL of a mixture of 0.1% formic acid acetonitrile and water with a volume ratio of 2:3 to test tube I to make up to volume, add 0.5mL acetonitrile to test tube to make up to volume, ultrasonicate for 30s, vortex mi...

Embodiment 3

[0070] Take the above-mentioned salmon and detect its veterinary drug residue content, the steps are as follows:

[0071] (1) Extraction: Weigh 3.0 g of uniformly prepared sample into a 50 mL centrifuge tube, add 15 mL of 1% acetic acid acetonitrile solution, vibrate vigorously for 1 min, ultrasonically extract for 20 min, and centrifuge at 4000 r / min for 5 min;

[0072] (2) Purification: transfer all the acetonitrile extracts obtained after centrifugation in step (1) to a mixed filler (10g anhydrous sodium sulfate, 500mgC 18 and 200mgPSA), vortexed for 1min, centrifuged at 4000r / min for 5min, accurately pipette 5.0mL supernatant to 10mL graduated test tubes I and II with stoppers, and concentrated to near dryness by nitrogen blowing in a water bath at 45°C , add 0.5mL of a mixture of 0.1% formic acid acetonitrile and water with a volume ratio of 2:3 to test tube I to make up to volume, add 0.5mL acetonitrile to test tube to make up to volume, ultrasonicate for 30s, vortex mix...

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Abstract

The invention belongs to the technical field of food detection methods, and particularly relates to a method for determining multiresidue of veterinary drugs in animal-derived foods. The method comprises the following steps of weighing a sample, adding an acetic acid-acetonitrile solution, carrying out vibrating extraction, centrifuging to obtain acetonitrile extracting solution, loading the extracting solution obtained by centrifuging into a centrifuge tube with a mixed filler, carrying out vibrating centrifugation, sucking purified liquid, concentrating by blowing nitrogen, diluting to constant volume and detecting by UPLC / MS / MS (ultra performance liquid chromatography-tandem mass spectrometry). The method disclosed by the invention is firstly applied in detecting animal-derived foods and 107 kinds of veterinary drugs such as sulfonamides, quinolones, beta agonists in animal products are subjected to fast qualitative and quantitative detection, the detection limit is completely capable of meeting the detection requirements and the detection efficiency is greatly promoted.

Description

technical field [0001] The invention belongs to the technical field of food detection methods, and in particular relates to a method for determining multiple residues of veterinary drugs in animal-derived foods. Background technique [0002] In 2003, Anastassiades and Lehotay developed a fast (quick), simple (easy), cheap (cheap), efficient (effective), durable (rugged) and safe (safe) sample pretreatment method for pesticide residues in agricultural products, And use the acronym to name this method QuEChERS. Since its release, QuEChERS has been widely adopted by many international pesticide residue analysis institutions including the American Association of Official Analytical Chemists (AOAC) because it simplifies the previous complicated extraction steps and expands the scope of the extracted pesticide residues. The field of residues finds a large number of applications. In the field of veterinary drug residues, the application of QuEChERS in the field of veterinary drug...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 宫明杰张禧庆郭海霞
Owner 烟台杰科检测服务有限公司
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