引用本文:王静, 周菁清.高效液相色谱串联质谱法直接测定环境水样中8种有机磷农药[J].环境监控与预警,2022,14(5):54-59
WANG Jing, ZHOU Jing-qing.Determination of 8 Organophosphorus Pesticides in Environmental Water Samples by High Performance Liquid Chromatography Tandem Mass Spectrometry[J].Environmental Monitoring and Forewarning,2022,14(5):54-59
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高效液相色谱串联质谱法直接测定环境水样中8种有机磷农药
王静, 周菁清
浙江省生态环境监测中心,浙江省生态环境监测预警及质控研究重点实验室,浙江 杭州 310012
摘要:
建立了一种高效液相色谱-串联质谱法(LC-MS/MS)同时测定环境水样中8种有机磷农药的分析方法。以地表水、地下水、污水和废水样品作为代表性水样基底,前处理方法仅采用简单的滤膜过滤,在C18柱分离后,在多反应监测模式下进行分析检测。结果表明,敌百虫、毒死蜱等有机磷农药在样品保存过程中迅速发生降解,分析须在样本采集后1 d内完成;该方法的检出限为0.10~0.20 μg/L,线性拟合相关系数(r)均>0.995;不同基底、不同浓度的加标回收实验表明,8种有机磷农药在环境基底中的回收率为74.5%~118%,相对标准偏差为0.4%~8.6%。该方法操作简便、灵敏度高、准确性好,在未来环境监测工作中具有较好的应用前景。
关键词:  有机磷农药  高效液相色谱串联质谱法  环境水样  检测方法
DOI:
分类号:X832
基金项目:浙江省生态环境科研和成果推广基金资助项目(2021XM0006)
Determination of 8 Organophosphorus Pesticides in Environmental Water Samples by High Performance Liquid Chromatography Tandem Mass Spectrometry
WANG Jing, ZHOU Jing-qing
Zhejiang Ecological and Environmental Monitoring Center, Zhejiang Key Laboratory of Ecological and Environmental Monitoring, Forewarning and Quality Control, Hangzhou, Zhejiang 310012, China
Abstract:
A high performance liquid chromatography tandem mass spectrometry (LC-MS/MS) method was developed for the simultaneous determination of eight organophosphorus pesticides in environmental water samples. Surface water, groundwater, and industrial and agricultural wastewater samples are selected as representative water matrix. Merely filter membrane filtration was used. After separation by C18column, analysis and determination were carried out in multiple reaction monitoring mode. The results showed that organophosphorus pesticides such as trichlorfon and chlorpyrifos were rapidly degraded during the sample storage, and the analysis should be completed within 1 day. The detection limits were in the range of 0.10 ~0.20 μg/L, and the linear fitting correlation coefficients were >0.995. Spiked recovery experiments on different substrates showed that the recoveries and RSDs ranged from 74.5% to 118% and 0.4% to 8.6%. The developed method is simple, sensitive and accurate, and has a good prospect of development and application in future environmental monitoring work.
Key words:  Organophosphorus pesticides  LC-MS/MS  Environmental water samples  Detection method