[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® 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.

[Determination of 64 veterinary drug residues in aquatic products by ultra-high performance liquid chromatography-quadrupole/electrostatic field orbitrap high-resolution mass spectrometry].

A method has been developed for the simultaneous determination of 64 veterinary drugs in aquatic products using ultra-high performance liquid chromatography-quadrupole/electrostatic field orbitrap high-resolution mass spectrometry. The samples were extracted with an acetonitrile/water mixture (80/20, v/v), cleaned up by normal hexane saturated with acetonitrile and primary secondary amine (PSA) adsorbent, quantified with external standard method. The drugs were analyzed in full scan/data dependent mass spectrum 2 (Full MS/ddMS2) Top 1 mode. The calibration curves of the 64 drugs were linear with the correlation coefficients more than 0. 9967. The average recoveries of the 64 analytes ranged from 56.2% to 124.6%, and the relative standard deviations (RSDs) were 1.3%-29.8% in the three kinds of matrixes (fish, shrimp and shell) at three levels. The limits of quantification were 0.2-10 µg/kg. The method is simple, rapid, sensitive, reliable and suitable for the screening of residues in aquatic products.