卢敏萍，黄克建，周哲，林翠梧*，杨宁，刘晓锋，高凡钦
单位
1.广西大学化学化工学院；2.广西壮族自治区公安厅物证鉴定中心；3.赛默飞世尔科技(中国)有限公司；4.广西高校应用化学技术与资源开发重点实验室；5.西安力邦医药科技有限责任公司
基金项目:质检公益性行业科研专项(2013,10143)
中文摘要:建立了同时测定全血、尿液和肝组织等生物样品中18种氨基甲酸酯类农药的在线固相萃取/液相色谱-线性离子阱质谱(On-line SPE/LC-LIT/MS)分析方法。样品经乙腈处理，稀释和离心后直接进样。经Waters Oasis? HLB在线SPE柱富集纯化，以BETASIL C18柱为分析柱，甲醇-水(均含0.1%甲酸)为流动相进行梯度洗脱；使用电喷雾电离(ESI)正离子模式测定，扫描方式为选择反应监测(SRM)和连续反应监测(CRM)。18种农药在考察的质量浓度范围内线性关系良好(权重因子1/X)，相关系数为0.9943~0.9994；在全血和尿液中的检出限为0.1~5 ng/mL，在肝组织中的检出限为0.1~5ng/g；3个加标水平的回收率为90.2%~114.5%，相对标准偏差(n=4)为0.5%~7.5%。该方法简单准确，灵敏度高，能够满足生物样品中18种氨基甲酸酯类农药的快速分析要求。
中文关键词:在线固相萃取 液相色谱-线性离子阱质谱法 连续反应监测(CRM) 氨基甲酸酯类农药 生物样品
Simultaneous Determination of Eighteen Carbamate Pesticides in Biological Samples by On-line Solid Phase Extraction Coupled with Liquid Chromatography-Linear Ion Trap Mass Spectrometry
Abstract:A new and sensitive analytical method was developed for the simultaneous determination of eighteen carbamate pesticides in biological samples by on-line solid phase extraction(on-line SPE) coupled with liquid chromatography-linear ion trap mass spectrometry(LC-LIT/MS).The samples were treated with acetonitrile,followed by dilution and centrifugation.The resulting solution was injected into LC system directly and processed with an Waters Oasis? HLB On-line SPE column for enrichment and purification.Separation was performed on a BETASIL C18 column with mixed mobile phases of methanol and water(both containing 0.1% formic acid) by gradient elution.The analytes were detected in selected reaction monitoring(SRM) or consecutive reaction monitoring(CRM) mode through positive electrospray ionization(ESI+).The calibration curves were linear within the investigated mass concentration ranges of the analytes(weighted 1/X),with correlation coefficients(r2) of 0.9943-0.9994.The LODs were in the ranges of 0.1-5ng/mL for whole blood and urine,and 0.1-5ng/g for liver tissue.The recoveries at three spiked levels ranged from 90.2% to 114.5%,with RSDs(n=4) of 0.5%-7.5%.The developed method is simple and accurate,and is sensitive for the rapid determination of eighteen carbamate pesticides in biological samples.
Key Words:on-line solid phase extraction(on-line SPE) liquid chromatography-linear ion trap mass spectrometry(LC-LIT/MS) consecutive reaction monitoring(CRM) carbamate pesticides biological samples
引用本文：卢敏萍，黄克建，周哲，林翠梧*，杨宁，刘晓锋，高凡钦.在线固相萃取/液相色谱-线性离子阱质谱法同时检测生物样品中18种氨基甲酸酯类农药[J].分析测试学报,2016,35(7):777-784.
