Citation: DONG Chanchan, HU Yanyun, LÜ Yaning, SONG Wei, HAN Fang, ZHENG Ping, DENG Ning. 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[J]. Chinese Journal of Chromatography, ;2016, 34(9): 850-859. doi: 10.3724/SP.J.1123.2016.04039 shu

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 Chanchan ^1, ,
HU Yanyun ^2,4 ,
LÜ Yaning ^2,3 ,
SONG Wei ^2,3 ,
HAN Fang ^2,3 ,
ZHENG Ping ^2,3 ,
DENG Ning 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 Date: 27 April 2016

Fund Project: Provincial Natural Science Foundation of Anhui, China (No. 1408085MKL97)

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.
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