气相色谱串联质谱法检测饮用水中酰胺类除草剂残留

刘存卫; 梁晓聪; 郭蓉; 田丽; 王玮

doi:10.13421/j.cnki.hjwsxzz.2021.01.018

气相色谱串联质谱法检测饮用水中酰胺类除草剂残留

Determination of Amide Herbicide Residues in Drinking Water by Gas Chromatography-Tandem Mass Spectrometry

摘要

摘要:
目的建立固相萃取—气相色谱串联质谱法检测饮用水中毒草胺、二甲吩草胺、乙草胺、甲草胺、杀草丹、异丙甲草胺、丁草胺和丙草胺8种酰胺类除草剂的方法。
方法水样经过活化后的C₁₈固相萃取柱，用乙腈-甲苯（3∶1，V/V）混合溶液洗脱，利用DB-5 MS石英毛细管柱分离，气相色谱串联质谱仪在多反应监测模式（MRM）下定性定量分析。
结果 8种酰胺类除草剂在（1.0~200）μg/L范围内线性关系良好，相关系数在0.999以上，方法检出限在（0.14~0.32）ng/L之间。在3个加标浓度水平（0.005、0.025和0.1 μg/L）下，回收率为75.8%~106.6%，相对标准偏差（RSD）为1.3%~6.2%。将建立的方法应用于实际样品的检测，水样中可检出目标物。
结论该方法简单快速，灵敏度和准确度高，能满足生活饮用水中常见酰胺类除草剂的检测。

Abstract:
Objective To establish a method for determining propachlor, dimethenamid, acetochlor, alachlor, benthiocarb, metolachlor, butachlor, and pretilachlor in drinking water by solid-phase extraction and gas chromatography-tandem mass spectrometry (GC-MS/MS).
Methods The water samples were extracted by an activated C₁₈ solid-phase column, eluted by acetonitrile-toluene (3∶1, V/V) mixed solution, and then separated by DB-5 MS quartz capillary column, and qualitative and quantitative analyses were performed by GC-MS/MS in multiple reaction monitoring mode.
Results The eight amide herbicides showed a good linear relationship ranged from 1.0 μg/L to 200 μg/L, with a correlation coefficient above 0.999, and the detection limit of this method ranged from 0.14 to 0.32 ng/L. At three spiked concentration levels (0.005, 0.025, and 0.1 μg/L), the recoveries ranged from 75.8% to 106.6%, and the relative standard deviation ranged from 1.3% to 6.2%. This method was applied to the detection of samples, and amide herbicides were detected in water samples.
Conclusion The method is simple, rapid, sensitive, and accurate and can be used for the detection of common amide herbicides in drinking water.

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