Detection method of residual quantities of various veterinary drugs in culturing or slaughtering environment

A determination method and technology of veterinary drug residues, which is applied in the field of determination of various veterinary drug residues in the breeding or slaughtering environment, can solve the difficulties in instrument detection setting, different chemical properties, and it is difficult to use the same pretreatment method and instrument detection for antibiotics Methods and other issues

Inactive Publication Date: 2012-04-25
ANIMAL AND PLANT & FOOD DETECTION CENTER JIANGSU ENTRY EXIT INSPECTION AND QUARANTINE BUREAU
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

However, some of these drugs, such as aminoglycosides, belong to a class of compounds with high polarity, and it is difficult to use the same pretreatment method and instrument detection method as other classes of antibiotics; nitrofurans need to determine their metabolites, and acid Hydrolyzed and derivatized, so it can only be classified and detected separately
The detection of other antibiotics such as lactams, tetracyclines, chloramphenicol, macrolides, lincosamides, sulfonamides and quinolones is mostly limited to one or several types of antibiotics at the same time. This is because different types of veterinary drugs have different polarities and different chemical properties, so it is difficult to simultaneously extract, purify, and detect residues of multiple types of veterinary drugs; There are also certain difficulties

Method used

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  • Detection method of residual quantities of various veterinary drugs in culturing or slaughtering environment
  • Detection method of residual quantities of various veterinary drugs in culturing or slaughtering environment
  • Detection method of residual quantities of various veterinary drugs in culturing or slaughtering environment

Examples

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example 1

[0014] Example 1 Detection of multiple veterinary drug residues in environmental water samples

[0015] Accurately take 100 mL of water sample filter paper into a clean glass Erlenmeyer flask, add 50 μL of mixed internal standard solution, add 50 mL of phosphate buffer solution, adjust the pH of the solution to 6.5, and vortex to mix. Use 6ml of methanol and 6mL of water to activate the OasisHLB column, pass the pH-adjusted sample solution through the column, and control the flow rate at 1-2d / s. After the flow is over, wash the centrifuge tube and the storage tube with 5mL of water and pass through the column. effluent. Under a negative pressure of 65kPa, vacuum dry for 10min, and finally elute with 6mL of methanol, collect the eluate in a 10mL test tube, dry it with a nitrogen blower at 45°C, and wash it with methanol+water (1+9v / v ) to 1.0 mL, pass through a 0.45 μm organic-phase nylon filter membrane into a sampling bottle for determination by liquid chromatography-mass sp...

example 2

[0016] Example 2. Detection of multiple veterinary drug residues in soil samples

[0017] Accurately weigh 10g (±0.05g) of the soil sample into a 500mL centrifuge tube, add 50μL of the mixed internal standard solution, add 200mL of phosphate buffer to adjust the pH of the solution to about 6.5, oscillate on the oscillator for 30min, filter the extraction solution In a clean 500mL Erlenmeyer flask. Use 6mL methanol and 6mL water to activate the Oasis HLB column, pass the filtered sample solution through the column, the flow rate is controlled at 1-2d / s, after the flow is over, wash the centrifuge tube and the storage tube with 6mL water and pass through the column. Under a negative pressure of 65kPa, vacuum dry for 10min, and finally elute with 5mL of methanol, collect the eluate in a 10mL test tube, dry it with a nitrogen blower at 45°C, and wash it with methanol+water (30+70v / v ) to 1.0 mL, pass through a 0.45 μm filter membrane into a sampling bottle for determination by li...

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Abstract

The invention provides a detection method of residual quantities of various veterinary drugs in a culturing or a slaughtering environment. With the method, rapid screening and quantitative detection can be carried out upon 61 drugs of 9 categories. The drugs include chlormycetin, beta lactams (penicillins), quinolones, sulfonamides, trimethoprims, macrolides, tetracyclines, and nitroimidazoles. According to the invention, a soil sample or an environmental water sample is added into a phosphate buffering solution; a filtrate obtained through centrifugation is extracted in a solid phase extraction column, and is eluted; the extraction column is dried by blowing, and is washed by using a methanol solution; an obtained eluent is titrated by using a methanol solution; a chromatogram peak of the sample is detected by using liquid chromatography-tandem mass spectrometry; the chromatogram peak is compared with a standard chromatogram peak, such that a specific variety of the detected drug is accurately determined. According to the invention, the sample solution is subject to liquid chromatography-tandem mass spectrometry multi-reaction monitoring selected ion analysis. Through internal standard correction, the recovering rate is 70-120%, and a relative standard deviation RSD is no larger than 18%. Compared with existing technologies, the analysis efficiency is improved by at least 5 times, and the detection cost is 30% of that of existing technologies.

Description

technical field [0001] The present invention relates to the simultaneous qualitative and quantitative determination of multiple veterinary drug residues in water bodies or soil samples that may be polluted by multiple antibiotics, specifically in the breeding or slaughtering environment of cattle, sheep, pigs, chickens, fish or shrimps, A variety of veterinary drugs including chloramphenicol, β-lactams (penicillins), quinolones, sulfonamides, sulfonamide synergists, macrolides, tetracyclines, nitroimidazoles, penicillins, a total of 9 There are 61 kinds of drugs in major categories. Background technique [0002] In recent years, due to the massive abuse and overuse of various veterinary drugs in the process of animal breeding, especially in the breeding or slaughtering of cattle, sheep, pigs, chickens, fish and shrimps, the soil and environmental water where the breeding or slaughtering is carried out have occurred. Indirect pollution. At present, the multi-residue determi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 蒋原薛峰丁涛张睿
Owner ANIMAL AND PLANT & FOOD DETECTION CENTER JIANGSU ENTRY EXIT INSPECTION AND QUARANTINE BUREAU
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