分散固相萃取-超高效液相色谱串联质谱法同时测定水产品中4种PPCPs

建立了分散固相萃取-超高效液相色谱串联质谱（dSPE-UPLC-MS/MS）测定水产品中磺胺甲基异恶唑（SMZ）、甲氧苄啶（TMP）、泰乐菌素（TYL）和三氯卡班（TCC）等两类4种PPCPs残留的分析方法。样品经乙腈提取，中性氧化铝吸附剂快速分散固相萃取净化，水浴条件下氮气吹干，20%乙腈-5 mM乙酸铵水溶液（含0.1%甲酸）溶解，离心过膜，上机检测。以乙腈和5 mM乙酸铵（含0.1%甲酸）作为流动相，Waters BEH C₁₈色谱柱梯度洗脱分离，分时段多反应监测模式下同时定量和定性分析。采用空白基质匹配标准法定量，各种药物在相应的质量浓度范围内线性关系良好，相关系数（r2）大于0.9984；方法的检测限和定量下限分别为0.1×10-9~1.0×10-9和0.2×10-9~2.0×10-9；样品的平均加标回收率为71.8%~96.5%，相对标准偏差小于9.8%。该方法操作简便快速、灵敏、可靠，适用于水产样品中4种PPCPs的测定。

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.