Dispersive solid-phase extraction followed byultra-high performance liquid chromatography tandem mass spectrometry for determination of 4 kinds of PPCPs residues in aquatic products

A generic, reliable and sensitive multiresidue analytical method was developed and validated for determination of 2 classes of PPCPs including sulfamethoxazole (SMZ), trimethoprim (TMP), tylosin (TYL) and triclocarban (TCC) in aquatic products using dispersive solid-phase extraction (dSPE) method and ultra-high performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS).Samples were extracted with acetonitrile, and then the extracts were purified by dispersive solid-phase extraction using Alumina N-neutral as adsorbent.The purified extraction was dried under nitrogen gas in water bath, and re-dissolved in 20% acetonitrile-5 Mm ammonium acetate water solution (containing 0.1% formic acid) and then centrifuged and filtered before UPLC-MS/MS analysis.Excellent chromatography separation was performed on a Waters BEH C₁₈ column under gradient elution condition utilizing acetonitrile and 5Mm ammonium acetate solution as mobile phases.Qualitative and quantitative analysis of target compounds was accomplished simultaneously in multiple-period multiple reaction monitor mode (multiple-period MRM).The correlation coefficients of linear calibration curves were over 0.9984 in the corresponding concentration range.The limits of detection (LODs) and quantification (LOQs) were in the range of 0.1×10^-9~1.0×10^-9 and 0.2×10^-9~2.0×10^-9, respectively.The recoveries of spiked samples were between 71.8% and 96.5% with relative standard deviation (RSD) less than 9.8%.The developed method can be applied to the residues determination of 4 PPCPs in aquatic samples.