Chinese Journal of Chromatography ›› 2018, Vol. 36 ›› Issue (2): 125-135.DOI: 10.3724/SP.J.1123.2017.10002

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Rapid screening of 24 tranquillizer drugs in fish and fishery products by ultra-high performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectroscopy

LI Rong1, YANG Luqi1,2, ZHANG Pengyun1, LUO Yangdan1, ZHANG Pengjie1, GAO Yongqing2   

  1. 1. Inspection and Quarantine Technology Center, Zhongshan Entry-Exit Inspection and Quarantine Bureau, Zhongshan 528400, China;
    2. School of Food Science, Guangdong Pharmaceutical University, Zhongshan 528458, China
  • Received:2017-10-08 Online:2018-02-08 Published:2014-01-17
  • Supported by:

    Science and Technology Planning Project of Guangdong Province of China (Nos.2015A050502010, 2014A040401011);Social Public Welfare Major Project of Zhongshan City (No.2015B2295).

Abstract:

A method was developed for the simultaneous determination of 24 tranquillizer drugs in fish and fishery products using ultra-high performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry (UPLC-Q-Orbitrap HRMS). The samples were extracted with acetonitrile. Then, the extracts were concentrated, dissolved by 50% (v/v) methanol aqueous solution, cleaned up with hexane saturated by acetonitrile. The separation was performed on an ACQUITY UPLC® BEH C18 column (100 mm×2.1 mm, 1.7 μm) with the gradient elution using acetonitrile and water both containing 0.1% (v/v) formic acid as mobile phases. The drugs were analyzed by full MS scan/data dependent MS2 (Full MS/dd-MS2)(Top 1) mode by heating electrospray ion (HESI) source. The results were quantified by external standard method. The calibration curves of the 24 tranquillizer drugs were linear in their respective linear range, the decision coefficients (r2) were no less than 0.9968. The average spiked recoveries of the 24 tranquillizer drugs were 58.9%-122.9%, and the relative standard deviations (RSDs) were 0.1%-16.4% in the six kinds of fish and fishery products at three spiked levels. The limits of quantification (LOQs) of the 24 tranquillizer drugs were 0.1-5.0 μg/kg. The method is simple, rapid, sensitive, reliable and suitable for the screening of the 24 tranquillizer drugs in fish and fishery products.

Key words: fish and fishery products, quadrupole/electrostatic field orbitrap high resolution mass spectroscopy (Q-Orbitrap HRMS), tranquillizer drugs, ultra-high performance liquid chromatography (UPLC)

CLC Number: