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Improved method of pretreatment process of determination of residue of veterinary drug in livestock and poultry meat

A technology of animals and livestock in meat, which is applied in the field of improvement of the pretreatment process for the determination of veterinary drug residues in livestock and poultry meat, can solve the problems of limited effective contact specific surface area, low drug extraction rate, poor dispersion of poultry meat, etc., and achieves improved The effective contact specific surface area and the effect of improving the extraction rate

Inactive Publication Date: 2019-04-05
江苏权正检验检测有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing determination method first dehydrates the sample and then extracts with an organic solvent or directly adds an organic solvent for extraction, but the poultry meat itself has poor dispersion and the effective contact specific surface area is limited, so the extraction rate of drug residues is low

Method used

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  • Improved method of pretreatment process of determination of residue of veterinary drug in livestock and poultry meat

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Embodiment 1

[0016] The present invention provides the following technical scheme: an improved method for the pretreatment process of determination of veterinary drug residues in livestock and poultry meat, comprising the following steps:

[0017] A. Weigh 4.98g sample, add 10ml deionized water to a 50mL stoppered centrifuge tube, and homogenize for 5min;

[0018] B. Add 20 mL of acidified acetonitrile, vortex for 1 min, and place in the dark for 10 min; add 30 g of anhydrous magnesium sulfate, centrifuge at 4 000 r / min for 5 min, and take the supernatant in a 100 ml centrifuge tube;

[0019] C. Add 10mL acidified acetonitrile to the residue to repeat the extraction once, combine the two extracts, and after purification, blow with nitrogen in a water bath at 40°C until dry;

[0020] D. Add 1.0 mL of methanol solution, vortex to dissolve the residue, pass through a 0.2 µm filter membrane, and use it for determination by liquid chromatography tandem mass spectrometer.

[0021] E. Repeat ste...

Embodiment 2

[0024] An improved method for the pretreatment process of the determination of veterinary drug residues in livestock and poultry meat, comprising the following steps:

[0025] A. Weigh 5.02 g of sample, add 10 ml of deionized water to a 50 mL centrifuge tube with stopper, and homogenize for 8 minutes;

[0026] B. Add 30 mL of acidified acetonitrile, vortex for 2 minutes, and place in the dark for 10 minutes; add 30 g of anhydrous magnesium sulfate, centrifuge at 5000r / min for 8 minutes, and take the supernatant in a 100ml centrifuge tube;

[0027] C. Add 10mL acidified acetonitrile to the residue to repeat the extraction once, combine the two extracts, and after purification, blow with nitrogen in a water bath at 40°C until dry;

[0028] D. Add 1.0 mL of methanol solution, vortex to dissolve the residue, and pass through a 0.2 µm filter membrane for determination by liquid chromatography tandem mass spectrometer.

[0029] E. Repeat steps A-D for determination.

[0030] Among...

Embodiment 3

[0032] An improved method for the pretreatment process of the determination of veterinary drug residues in livestock and poultry meat, comprising the following steps:

[0033] A. Weigh 4.99g sample, add 10ml deionized water to a 50mL stoppered centrifuge tube, and homogenize for 5min-8min;

[0034] B. Add 22 mL of acidified acetonitrile, vortex for 1 min, and place in the dark for 10 min; add 30 g of anhydrous magnesium sulfate, centrifuge at 4200r / min for 6 min, and take the supernatant into a 100ml centrifuge tube;

[0035] C. Add 10 mL of acidified acetonitrile to the residue to repeat the extraction once, combine the two extracts, and after purification, blow with nitrogen in a water bath at 40°C until dry;

[0036] D. Add 1.0mL methanol solution and vortex to dissolve the residue, pass through a 0.2µm filter membrane for determination by liquid chromatography tandem mass spectrometer.

[0037] E. Repeat steps A-D for determination.

[0038] Among them, the production me...

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Abstract

The invention discloses an improved method of the pretreatment process of determination of residue of veterinary drug in livestock and poultry meat. According to the improved method, an attenuation step and a homogeneity step are added before acetonitrile extraction is carried out, the problems that the livestock and poultry meat is not easy to disperse and the to-be-tested drug residue is not easy to extract are solved, the effective contact specific surface area between a to-be-tested sample and an extraction solvent is increased greatly, and thus the extraction ratio of to-be-tested drug residue components is improved significantly.

Description

technical field [0001] The invention relates to the technical field of determination of veterinary drug residues, in particular to an improved method for the pretreatment process of determination of veterinary drug residues in livestock and poultry meat. Background technique [0002] Eating a large amount of food containing drug residues will cause the gradual accumulation of drugs in the human body, which will cause urinary system and digestive system damage, thrombocytopenia, allergic reactions, and lead to bacterial drug resistance and carcinogenic effects. Governments of various countries have strictly regulated the maximum residue limit (MRL) of veterinary drugs used in animal food. [0003] At present, there are many methods for the determination of veterinary drug residues, the most common method is liquid chromatography tandem mass spectrometry. The key to this method is the effective extraction of the analyte in the pretreatment of the sample. There are many steps...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/14G01N30/72
CPCG01N30/02G01N30/06G01N30/14G01N30/72G01N2030/027G01N2030/062G01N2030/146
Inventor 张荣荣邓飞燕巩长海
Owner 江苏权正检验检测有限公司