Detection method for veterinary drug residues

A detection method, a technology for veterinary drug residues, applied in the field of detection of veterinary drug residues, can solve the problems of low sensitivity, cumbersome pretreatment, and difficulty in analyzing multiple components at the same time, and achieve the effect of high sensitivity and strong specificity

Inactive Publication Date: 2014-04-30
CHINA ANIMAL DISEASE CONTROL CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But it also has many defects: high selectivity to reagents, it is difficult to analyze multiple components at the same time; there is a certain degree of cross-reaction to compounds with similar structures; there is a certain degree of difficulty in analyzing compounds with small molecular weight or very unstable compounds. difficulty
[0009] The methods in the prior art often have problems such as low sensitivity, cumbersome pretreatment, single detection drug or poor reproducibility, and it is difficult to meet the simultaneous confirmation detection of drug residues.

Method used

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  • Detection method for veterinary drug residues
  • Detection method for veterinary drug residues
  • Detection method for veterinary drug residues

Examples

Experimental program
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Effect test

Embodiment 1

[0079] 1 Instruments and reagents

[0080] 1.1 Instrument

[0081] Waters Ultra Performance LC liquid chromatograph (Waters Company), Quattro Premier XE mass spectrometer (Waters Company), MassLynx v4.1 data processing software (Waters Company); Waters Acquity UPLC BEH C 18 Chromatographic column (100mm×2.1mm, 1.7μm); TranssonicTP690 ultrasonic cleaner (Elma Company); 3K15 centrifuge (Sigma Company); Millipore Elix Milli-Q pure water instrument.

[0082] 1.2 Materials

[0083] Chromatographically pure methanol (product of Fisher Scientific); chromatographically pure acetonitrile (product of Fisher Scientific); ultrapure water; other reagents were of analytical grade.

[0084] The 46 drugs used were all commercially available, and the purity of each drug was higher than 98.0%.

[0085] Healthy beef (determined not to contain any of the 46 drugs) was quantitatively added to the tetracycline, oxytetracycline, chlortetracycline, doxycycline, terbutaline, cimaterol, salbutamol, ...

Embodiment 2

[0120] Healthy beef (not containing any one of the 46 kinds of drugs after testing) was added 2.0mL of the mixture of tetracycline, oxytetracycline, aureomycin and doxycycline (concentration: 10ng / ml). After the drug is added, the beef is first fully pulverized with a cooking machine and stored in a freezer; accurately weigh 5.0g of thawed beef, put it in a 50mL centrifuge tube, add 10% trichloroacetic acid: acetonitrile extract (V: V=20 : 80) 10.0mL, fully homogenized, ultrasonically extracted for 10min, 10000r·min -1 After centrifugation for 10 min, the supernatant was transferred to another 50 mL centrifuge tube, and the residue was extracted once more with 10.0 mL of extraction solution. The extracts were combined, and the extract was blown dry at 30°C with nitrogen. The residue was dissolved with 2.0 mL of the initial mobile phase, vortexed and mixed at 10000 r min -1 Centrifuge at high speed for 10 min. Take an appropriate amount of supernatant, filter it with a 0.45 ...

Embodiment 3

[0126] Add 0.5mL of the 10 kinds of β-receptor agonist drug mixture and 3 kinds of deuterated internal standards to the healthy beef (which is determined not to contain any of the 46 kinds of drugs) according to each gram of beef Mixture (concentration of 10ng / ml). After the drug is added, the beef is first fully pulverized with a cooking machine, and stored in a freezer; accurately weigh 5.0g of thawed beef, put it in a 50mL centrifuge tube, add 10% trichloroacetic acid: acetonitrile extract (V: V=25 : 75) 10.0mL, fully homogenized, ultrasonically extracted for 10min, 9000r·min -1 After centrifugation for 12 min, the supernatant was transferred to another 50 mL centrifuge tube, and the residue was extracted once more with 10.0 mL of extraction solution. The extracts were combined and dried under nitrogen at 25°C. The residue was dissolved with 2.0 mL of the initial mobile phase, vortexed and mixed at 9000 r min -1 Centrifuge at high speed for 12 minutes. Take an appropriat...

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Abstract

The invention provides a detection method for veterinary drug residues. The detection method comprises the following steps of (1) treating a sample: pretreating the sample to be detected, adding an extracting agent, and performing treatment by multiple steps to obtain supernate, wherein filtrate obtained by filtration on the supernate is used for UPLC-MS / MS (ultra performance liquid chromatography-mass spectrum / mass spectrum) measurement; (2) measuring the veterinary drug residues: performing UPLC-MS / MS measurement on the obtained sample under a certain measurement condition. The detection disclosed by the invention has the characteristics of high sensitivity and high specificity and can conform to the detection on the veterinary drug residues.

Description

technical field [0001] The invention relates to a detection method, in particular to a detection method for veterinary drug residues. Background technique [0002] Veterinary drugs play a very important role in preventing and controlling animal diseases, increasing production efficiency, and improving the quality of animal products. However, due to the lack of scientific knowledge and the blind pursuit of economic interests by the breeders, the abuse of veterinary drugs is common in the current animal husbandry. [0003] With the transformation of people's demand for animal-sourced foods to quality-based ones, veterinary drug residues in animal-sourced foods have gradually become a focus of attention all over the world. Veterinary drug residues refer to the prototype drug or its metabolites that accumulate or remain in livestock and poultry bodies or products (such as eggs, milk, meat, etc.) after medication, including residues of impurities related to veterinary drugs. At...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 王海田亚平姜艳彬单吉浩
Owner CHINA ANIMAL DISEASE CONTROL CENT
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