全自动在线固相萃取-液相色谱串联质谱法快速测定地表水中痕量甲基对硫磷  

Fully automated on-line solid phase extraction coupled with liquid chromatography tandem mass spectrometry for rapid determination of trace methyl parathion in surface water

作　　者：任颖俊 彭君 赵锦华 刘立平 李超群 梁锋 REN Yingjun;PENG Jun;ZHAO Jinhua;LIU Liping;LI Chaoqun;LIANG Feng(Hunan Geological Experiment and Testing Center,Changsha,410007,China)

机构地区：[1]湖南省地质实验测试中心,长沙410007

出　　处：《环境化学》2024年第7期2504-2507,共4页Environmental Chemistry

基　　金：湖南省自然资源厅科技项目(2022B03);湖南省地质院科研基金(HNGSTP202214)资助.

摘　　要：建立了全自动化在线固相萃取-液相色谱串联质谱法快速、准确测定地表水中痕量甲基对硫磷的方法.水样经在线富集、色谱柱分离后,梯度洗脱,采用电喷雾离子源正离子多反应监测模式,内标法定量.通过对离子源参数、水相洗脱溶剂、有机相洗脱溶剂、洗脱溶剂初始比例进行优化试验,甲基对硫磷的灵敏度显著提升,峰型更好.该方法在质量浓度5—1000 ng·L^(-1)范围内线性关系良好(相关系数R^(2)≥0.998).添加回收试验结果表明,方法检出限为4 ng·L^(-1),方法定量限为16 ng·L^(-1),在40、100、500 ng·L^(-1)的3个添加水平下,平均回收率为90.1%—97.8%,相对标准偏差为1.7%—3.5%。应用于实际地表水样品测定,结果均未检出.该方法便捷、高效,可实现高通量测定地表水中痕量甲基对硫磷.A method for rapid and accurate determination of trace methyl parathion in surface water by Fully automated on-line solid phase extraction coupled with liquid chromatography tandem mass spectrometry was established.The water samples were enriched online,separated on a chromatographic column with gradient elution,and quantified by internal standard method using electrospray ionization source in positive ions multiple reaction monitoring mode.By optimizing the ion source parameters,changing aqueous phase eluent,organic phase eluent,and initial ratio of eluent,the sensitivity of methyl parathion was significantly improved,and the peak shape got better.The method showed good linearity in the mass concentration range of 5—1000 ng·L^(-1)(Correlation coefficient(R^(2))≥0.998).Through standard addition experiments,The results showed that the limit of detection of the method was 4 ng·L^(-1) and the limit of quantification was 16 ng·L^(-1).The average recovery at 3 addition concentrations of 40,100,and 500 ng·L^(-1) was 90.1%—97.8%,with a relative standard deviation(RSD)of 1.7%—3.5%.The method was applied to the determination of actual surface water samples,and no trace of methyl parathion was detected.The method is convenient and efficient,and can achieve high-throughput determination of trace methyl parathion in surface water.

关 键 词：全自动在线固相萃取 液相色谱 串联质谱 甲基对硫磷 

分 类 号：X-1[环境科学与工程] O6[理学—化学]