全自动在线HS-SPME-GC-MS/MS检测鱼塘投毒案件水样中的13种有机磷农药  

Detection of 13 organophosphorus pesticides in fishpond water of poisoning cases by automatic online HS-SPME-GC-MS/MS

作　　者：王丹[1] 宋歌[2] 姜红[1] 董林沛 赵鹏[2] WANG Dan;SONG Ge;JIANG Hong;DONG Linpei;ZHAO Peng(School of Investigation,People’s Public Security University of China,Beijing 100038,China;Institute of Forensic Science,Ministry of Public Security,Beijing 100038,China)

机构地区：[1]中国人民公安大学侦查学院,北京100038 [2]公安部物证鉴定中心,北京100038

出　　处：《中国测试》2021年第3期70-75,共6页China Measurement & Test

基　　金：中央级公益性科研院所基本科研业务费项目(2019JB002)。

摘　　要：建立全自动在线顶空固相微萃取-气相色谱串联质谱技术(HS-SPME-GC-MS/MS)检测鱼塘投毒案件水样中13种有机磷农药的方法。将2 mL水样中加入0.6 g氯化钠(NaCl)置于20 mL顶空瓶中,使用直径为100μm的聚二甲基硅氧烷(PDMS)萃取纤维,在75℃条件下萃取45 min,采用GC-MS/MS多反应监测模式(MRM)进行检测。13种有机磷农药在线性范围内线性关系良好,标准曲线相关系数(r^(2))>0.99,方法检出限为0.002-0.5 ng/mL,定量限为0.006-1.8 ng/mL,精密度在1.92%-17.10%之间。该方法灵敏度高,并且操作简单,样品的处理与分析过程全自动进行,可提高工作效率,适用于鱼塘投毒案件水样中13种有机磷农药的检测。An automatic online headspace solid-phase microextraction-gas chromatography-tandem mass spectrometry(HS-SPME-GC-MS/MS)method was established to detect 13 organophosphorus pesticides in fishpond water.The optimum extraction conditions were as follows:0.6 g NaCl was added to 2 mL of aqueous solution sample in 20 mL headspace bottle,100μm PDMS fiber was used to extract the sample at 75℃ for 45 min,the analysis was performed by GC-MS/MS in multiple reaction monitoring mode(MRM).The correlation coefficients of the standard curves were above 0.99(r^(2)>0.99).The limits of detection(LODs)of 13 organophosphorus pesticides ranged from 0.002 to 0.5 ng/mL,and the limits of quantification(LOQs)ranged from 0.006 to 1.8 ng/mL,the precisions of the method were 1.92% to 17.10%.The method has high sensitivity,and the whole process can be carried out automatically,making it easy to operate.It is suitable for the detection of 13 organophosphorus pesticides in fishpond water.

关 键 词：顶空固相微萃取 气相色谱-串联质谱 鱼塘水 有机磷农药 

分 类 号：O657.63[理学—分析化学]