Chinese Journal of Chromatography

Chinese Journal of Chromatography ›› 2016, Vol. 34 ›› Issue (9): 850-859.DOI: 10.3724/SP.J.1123.2016.04039

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Magnetic graphene based dispersive micro-solid-phase extraction coupled with liquid chromatography-tandem quadrupole mass spectrometry for the analysis of nine non-steroidal anti-inflammatory drugs in livestock and poultry meat

DONG Chanchan1, HU Yanyun2,4, LÜ Yaning2,3, SONG Wei2,3, HAN Fang2,3, ZHENG Ping2,3, DENG Ning1   

  1. 1. School of Chemistry and Chemical Technology, Hefei University of Technology, Hefei 230009, China;
    2. Anhui Entry-Exit Inspection and Quarantine Bureau, Hefei 230022, China;
    3. Anhui Province Key Laboratory of Analysis and Detection for Food Safety, Hefei 230022, China;
    4. School of Public Health, Anhui Medical University, Hefei 230032, China
  • Received:2016-04-27 Online:2016-09-08 Published:2016-08-26
  • Supported by:

    Provincial Natural Science Foundation of Anhui, China (No. 1408085MKL97); State Quality Inspection Administration Science and Technology Projects (No. 2014IK134); Shanghai Yangtze River Science and Technology Cooperation Projects (No. 15395810100); Anhui Science and Technology Program (No. 1604b0602028).

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Abstract:

A novel analytical method was developed for the determination of nine non-steroidal anti-inflammatory drugs (NSAIDs) in meat samples by magnetic graphene nanocomposite (Fe3O4-G) based on dispersive micro-solid-phase extraction (μ-SPE) coupled with liquid chromatography-mass spectrometry detection. Samples were homogenized and extracted with acidified acetonitrile. After defatting with the high speed frozen centrifugation, the sample solutions were defatted with n-hexane followed by μ-SPE. Some important parameters influencing the extraction efficiency including the extraction time, the pH value of sample solution and the elution conditions were optimized. The limits of detection (LODs, S/N=3) of the nine NSAIDs ranged from 0.2 to 8.2 μg/kg, and the limits of quantification (LOQs, S/N=10) ranged from 0.5 to 25.4 μg/kg. The average recoveries were 83.3%-104.5% with the relative standard deviations between 1.2% and 6.8% obtained from samples spiked at LOQ, 2LOQ and 10LOQ levels. Compared with Sep-Pak Vac NH2 and Oasis HLB cartridges, Fe3O4-G has excellent purification effect, high loading amounts and good reusability. The results demonstrated that the method provide a novel pretreatment technique for the determination of NSAID residues in meat samples.

Key words: dispersive micro-solid-phase extraction, liquid chromatography-quadrupole mass spectrometry (LC-MS/MS), livestock and poultry meat, magnetic graphene nanocomposite, non-steroidal anti-inflamma-tory drugs

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