磁性固相萃取-液相色谱-质谱联用测定环境水中13种三嗪类除草剂  

Determination of 13 Triazine Herbicides in Environmental Water by Magnetic Solid Phase Extraction with High-performance Chromatography-mass Spectrometry

作　　者：刘翔[1] 滕姣 周艳 梁俊阳 陈学国[3] LIU Xiang;TENG Jiao;ZHOU Yan;LIANG Jun-yang;CHEN Xue-guo(Graduate School,Criminal Investigation Police University of China,Shenyang Liaoning 110035;Deparment of Criminal ldenification,Guangdong Justice Police Vocational College,Guangzhou Guangdong 510520;School of Forensic Science,Criminal Investigation Police University of China,Shenyang Liaoning 110035;Center of Material Evidence Identification,Jilin Public Security Bureau Changchun,Changchun Jilin 130051)

机构地区：[1]中国刑事警察学院研究生院,辽宁沈阳110035 [2]广东司法警官职业学院司法鉴定系,广东广州510520 [3]中国刑事警察学院刑事科学技术学院,辽宁沈阳110035 [4]吉林省公安厅物证鉴定中心,吉林长春130117

出　　处：《中国刑警学院学报》2022年第3期111-118,共8页Journal of Criminal Investigation Police University of China

基　　金：2020年度公安部刑事技术“双十计划”重点攻关任务立项项目(编号:2020SSGG0503);2020年度辽宁省教育厅科学研究经费项目(编号:2020191);2021年度辽宁省自然科学基金项目(编号:2021-MS-144)。

摘　　要：利用化学共沉淀法制备磁性固相萃取材料-磁性碳纳米管,结合液相色谱-电喷雾离子阱质谱联用分析技术,建立环境水中三嗪类除草剂的磁性固相萃取-液相色谱-质谱联用定性、定量分析方法。环境水中的分析物经磁性碳纳米管净化、提取和富集后,进行液相色谱-电喷雾离子阱质谱联用分析。结果表明,环境水中13种三嗪类除草剂在各自的浓度范围内线性关系良好,检出限小于0.005μg/mL,定量限小于0.01μg/mL,日内精密度小于7.64%,日间精密度小于9.54%,平均回收率为91.79%~98.60%。所建立的检测方法操作简便、绿色环保、检测灵敏,可应用于司法鉴定实践之中。Based on magnetic solid phase extraction and liquid chromatography-mass spectrometry,a method for qualitative and quantitative analysis of triazine herbicides in environmental water was developed.The analytes in environmental water were purified,extracted and enriched by magnetic carbon nanotubes,and then analyzed by liquid chromatography-mass spectrometry.The experimental results showed that in environmental water,the limited of detection (LOD) was less than 0.0005μg/mL.Limited of quantity (LOQ) was less than 0.001μg/mL.The average intra-day precision was less than 7.64%.The average inter-day precision was less than 9.54%,and the average recovery was between 91.79% and 98.60%,respectively.The experimental results and application in relevant case evidence inspection showed that this method was easy to operate,green,and efficient,and could provide scientific basis for case physical evidence identification.

关 键 词：磁性碳纳米管 固相萃取 液相色谱-质谱 三嗪类除草剂 环境水 

分 类 号：O657.63[理学—分析化学]