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Simultaneous Determination of Residues of Four Dipyrone Metabolites in Goat Muscle by Hydrophilic Interaction Liquid Chromatography-Mass Spectrometry

ZHANG Chong1,2, XUE Fei-qun2, ZHANG Li-fang2, ZHANG Xiao-xiao2, WANG Xiao-yang2, JIANG Shan-xiang1,*   

  1. 1. Laboratory of Veterinary Pharmacology and Toxicology, College of Veterinary Medicine, Nanjing Agricultural University,
    Nanjing 210095, China; 2. Key Laboratory of Veterinary Drug Safety Evaluation and Residue Research,
    Shanghai Veterinary Research Institute, Chinese Academy of Agricultural Sciences, Shanghai 200241, China
  • Online:2014-05-25 Published:2014-05-29
  • Contact: JIANG Shan-xiang

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Abstract:

A hydrophilic interaction liquid chromatography-mass spectrometry (HILIC-MS) method was developed for
the determination of four dipyrone metabolites, namely 4-methylaminoantipyrine (MAA), 4-aminoantipyrine (AA),
4-formylaminoantipyrine (FAA), and 4-acetylaminoantipyrine (AAA) in goat muscle. These metabolites were extracted with
acetonitrile mixed with 5% ammonia. The extracts were cleaned up with Cleaner PSA, and then blow-dried by nitrogen gas,
re-dissolved in acetonitrile and re-cleaned up using MAX (SPE) cartridge. After chromatographic separation, the analytes were
quantified by the external standard method. The calibration curves were linear between 4 and 200 μg/kg matrix equivalent
concentrations for MAA, FAA, and AAA, and between 40 and 2 000 μg/kg for AA. The mean recoveries in blank samples
at four spike levels (5, 50, 100, and 1 000 μg/kg) ranged between 75.02% and 116.2%. The intra-day coefficient of variation
(CV) was 1.63% to 15.12% (n = 5), and the inter-day CV was less than 11% (n = 15). The detection limits were 0.5 μg/kg
for MAA, FAA and AAA and 5 μg/kg for AA. The proposed method is sensitive and repeatable, allowing analysis of a large
number of samples in a working day.

Key words: goat muscle, dipyrone metabolites, hydrophilic interaction liquid chromatography coupled with tandem mass spectrometry

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