用液相色谱串联质谱法测定渔业水样中6种农药的含量

本文建立了一种快速检测渔业水质样本中酰胺类除草剂乙草胺、丙草胺、丁草胺、三嗪类除草剂莠去津、烟碱类杀虫剂噻虫嗪、三唑类杀菌剂苯醚甲环唑6种农药含量的液相色谱串联质谱法。采用乙腈-水-甲酸梯度洗脱、电喷雾电离方式、多反应监测模式测定考察检出限、线性范围、日内精密度及日间精密度。在三种加标浓度下,该方法的回收率为78.2%~104.7%。用液相色谱-四级杆-飞行时间质谱对疑似目标物质进行定性,用精确质量数、同位素丰度比和二级碎片解析方式等解析定性结构。该方法能够满足检测这六种农药的要求,能准确定性,自建的谱库可为渔业污染事故鉴定和水产品质量安全风险评估做支撑。

Detection of Six Pesticides in Fishery Waters by Liquid Chromatography Tandem Mass Spectrometry

A rapid detection method of six pesticides in fishery waters by liquid chromatography tandem mass spectrometry (LC-MS/MS) was established,including acetochlor,pretilachlor,butachlor,atrazine,thiamethoxam and difenoconazole.Mixtures of acetonitrile and 0.1％ (Φ) formic acid solution with different mixing ratio were used as eluants in the elution,and ESI+ mode was used,and multi-reaction monitoring mode was employed.The limit of detection,linear range and relative standard deviations of within-and between-day were investigated.In all three spiked levels recoveries of spiked samples were ranged from 78.2％ to 104.7％,and the suspected compounds were confirmed by liquid chromatography quadrupole time of flight mass spectrometry (LC-Q-TOFMS),due to its accurate mass,isotopic pattern and MS/MS.A simple solid-phase extraction method was applied to separate the six pesticides,and the analytes were detected by LC-MS/MS and LC-Q-TOFMS.This method was shown to be more accurate and qualitative,and the self-built library provides support for the assessment of fishery pollution accident,and quality and safety risk assessment of fishery products in future.