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

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

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。

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 5 Mm 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.