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

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 (R) BEH C-18 column (100 mm x 2.1 mm, 1.7 mu m) 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 (r(2)) were no less than 0.996 8. The aver. age spiked recoveries of the 24 tranquillizer drugs were 58.9%-122.9%, and the relative stand. ard 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 mu g/kg. The method is simple, rapid, sensitive, reliable and suitable for the screening of the 24 tranquillizer drugs in fish and fishery products.