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  

Simultaneous Determination of Eighteen Carbamate Pesticides in Biological Samples by On-line Solid Phase Extraction Coupled with Liquid Chromatography- Linear Ion Trap Mass Spectrometry

作　　者：卢敏萍 黄克建[2] 周哲 林翠梧[1,4] 杨宁[2] 刘晓锋[2] 高凡钦 

机构地区：[1]广西大学化学化工学院,广西南宁530004 [2]广西壮族自治区公安厅物证鉴定中心,广西南宁530012 [3]赛默飞世尔科技(中国)有限公司,上海201206 [4]广西高校应用化学技术与资源开发重点实验室,广西南宁530004 [5]西安力邦医药科技有限责任公司,陕西西安710065

出　　处：《分析测试学报》2016年第7期777-784,共8页Journal of Instrumental Analysis

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0.994 3～0.999 4;在全血和尿液中的检出限为0.1～5 ng/m L,在肝组织中的检出限为0.1～5 ng/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。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 in- jected into LC system directly and processed with an Waters Oasis HLB On-line SPE column for en- richment 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 investi- gated mass concentration ranges of the analytes（weighted 1/X）, with correlation coefficients （ r2 ） of 0. 994 3 - 0. 999 4. The LODs were in the ranges of 0. 1 - 5 ng/mL for whole blood and urine, and 0. 1 -5 ng/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.

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 

分 类 号：O657.63[理学—分析化学] F767.2[理学—化学]