4.5 Article

Development of a multi-residue method for fast screening and confirmation of 20 prohibited veterinary drugs in feedstuffs by liquid chromatography tandem mass spectrometry

Publisher

ELSEVIER SCIENCE BV
DOI: 10.1016/j.jchromb.2013.07.028

Keywords

Multiclass drugs; Liquid chromatography-tandem mass spectrometry; QuEChERS; Feed

Funding

  1. 973 Fund, the Ministry of Science and Technology of the People's Republic of China [2009CB118805]
  2. National Natural Science Foundation of China [31072166]

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A simple multiresidue method was developed for detecting and quantifying twenty analytes from 5 classes of prohibited veterinary drugs (beta-agonists (9), anabolic hormones (4), quinoxalines (4), tranquilizers (1), cyproheptadine, and clonidine in animal feeds using a QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) approach. Feed samples were extracted by ultrasonic-assisted extraction with a mixture of methanol-acetonitrile (50:50, v/v), followed by a cleanup using a dispersive solid-phase extraction with PSA (primary secondary amine). Target compounds were separated and determined by a liquid chromatography tandem quadrupole mass spectrometer operating in positive electrospray ionization mode, using multiple reaction monitoring (MRM). The recoveries of these compounds were between 56.7% and 103% at three spiked levels. The repeatability was lower than 10%, whereas reproducibility was no more than 15% except for nandrolone (17% at 10 mu g kg(-1)) and diazepam (19% at 10 mu g kg(-1)). Decision limits (CC alpha s) and detection capabilities (CC beta s) ranged from 0.42 to 5.74 mu g kg(-1) and 5.70-9.81 mu g kg(-1), respectively. The method was successfully applied to screening of real samples obtained from local feed markets and confirmation of the suspected target analytes. (C) 2013 Elsevier B.V. All rights reserved.

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