固相萃取-GC-MS/MS法测定海水中莠去津及其代谢物残留研究

采用固相萃取结合气相色谱-串联质谱(GC-MS/MS), 建立了海水中痕量莠去津(ATR)及其主要代谢产物脱乙基莠去津(DEA)、脱异丙基莠去津(DIA)和脱乙基脱异丙基莠去津(DDA)的精确定量分析方法. 海水样品在萃取前调节pH至3.0, 然后经HLB固相萃取柱富集、净化, 在GC- MS/MS多反应监测模式(MRM)下进行定性、定量分析, 并对该方法的线性、检出限、准确度和精密度进行验证分析. 结果表明: ATR、DEA、DIA和DDA在质量浓度为0.5~100.0μg?L-1范围内具有良好的线性相关性, R2均大于0.9990, 方法检出限依次为0.120、0.060、0.060、0.024ng?L-1, 回收率为92.3%~104.7%, 相对标准偏差(RSD)小于6.6%. 本文方法具有较好的线性、灵敏度、准确度和精密度, 并已成功应用于象山港海水实际样品的检测分析.

Determination of atrazine and its metabolites in seawater by solid phase extraction and gas chromatography tandem mass spectrometry (GC-MS/MS)

An accurate analytical method was developed for the determination of trace level of atrazine (ATR) and its major metabolites (deethylatrazine, DEA; deisopropylatrazine, DIA; didealkylatrazine, DDA) in seawater by coupling solid-phase extraction with gas chromatography tandem mass spectrometry (GC-MS/MS). The HLB solid-phase extraction (SPE) column was used to enrich and purify the target analytes in seawater. Furthermore, the parameters affecting the SPE extraction efficiency were optimized. The pH of the seawater sample was adjusted to 3 before the SPE extraction. Subsequently, the samples were analyzed by GC-MS/MS with multi-reaction monitoring mode (MRM), and the limit of detection (LOD), sensitivity, accuracy and precision were verified. Finally, the results indicated that the good linear relationship in the range of 0.5-100.0μg?L-1 with R2 above 0.9990 was obtained. The LODs of ATR, DEA, DIA and DDA were 0.12, 0.06, 0.06 and 0.024ng?L-1, respectively. The excellent recoveries of ATR, DEA, DIA and DDA were in the range of 92.3%-104.7% with RSD below 6.6%. The results demonstrated that the present method has optimal linearity, sensitivity, accuracy and precision. It could be successfully applied to the analysis of four analytes in the seawater samples from Xiangshan Bay.