仪器应用

固相微萃取与低热容气相色谱质谱联用快速分析水中有机磷农药残留量

陶芊

(安捷伦科技(上海)有限公司，上海 200131)

摘要：介绍了一种基于固相微萃取(SPME)技术和5975T低热容(LTM)GC/MS分离分析平台的水中有机磷农残快速测定方法。该方法选用细内径短柱，通过优化分离条件，5975T可在3min内完成对5种常见有机磷农药(毒死蜱，甲基异柳磷，喹硫磷 ，丙溴磷 ，伏杀硫磷)的分离鉴定，相比实验室常规分离方法用时节省90%，联用SPME其方法定量检出限优于5 ng/L。该方法的固相微萃取过程装置简单，操作简便，无需调节萃取体系的离子强度和pH值，20min完成富集，时间/物料成本低廉。同时，还考察了方法的线性范围、精密度和回收率，并对自来水管网水中农药残留进行了分析。

关键词：固相微萃取;低热容气质联用仪;有机磷农药;快速分离分析

作者简介：陶芊，男，1983年生，分析化学博士，主要从事分析仪器研发及相关应用方法开发，E-mail:taoqian@alu.fudan.edu.cn。

DOI:10.3936/j.issn.1001-232x.2015.01.004

收稿日期：2014-06-20

基金项目：国家自然科学

Fast analysis of organophosphorous pesticides in water by SPME and low thermal mass GC/MS.TaoQian(AgilentTechnologies(Shanghai)Co.,Ltd.,Shanghai, 200131,China)

Abstract:A fast method based on solid phase microextraction (SPME) technique and a brand-new analysis platform 5975T (low thermal mass GC/MS) for the analysis of organophosphorous pesticides (OPPs) in water was developed. By using a thin-bore and short column and optimizing the separation condition, 5 OPPs (dursban, isofenphos-methyl, quinalphos, profenofos, phosalone) were separated and identified with 5975T within 3 min, compared with conventional separeation methods to save time 90%. The limits of quantitation of OPPs in water were less than 5 ng/L. The concentration process of SPME was simple and costless. It can be completed in 20 min with no need of adjusting ionic intensity and pH valve. The linear range, repeatability and recovery of the method were studied. The OPPs in pipe water of Pudong district were determined.

Key words：solid phase microextraction (SPME); low thermal mass GC/MS; organophosphorous pesticides (OPPs); fast separation and analysis

1引言

第二次世界大战后，人工合成有机农药开始广泛应用于农业生产。到目前为止，我国每年农药的使用量约在100~130万吨[1]。有机磷农药是最常用的农药，多为磷酸酯类或硫代磷酸酯类，如敌敌畏、乐果、马拉硫磷、甲基对硫磷等。这些化合物有很强的毒性，被吸收后会抑制乙酰胆碱酯酶，使乙酰胆碱积聚，引起毒蕈碱样症状、烟碱样症状以及中枢神经系统症状，严重时可因肺水肿、脑水肿、呼吸麻痹而死亡，重度急性中毒者还会发生迟发性猝死；……