固相萃取-超高效液相色谱-三重四级杆质谱法测定农田水中15种氨基甲酸酯类农药

Determination of 15 carbamate pesticides in farmland water by solid phase extraction-ultra high performance liquid chromatography-triple quadrupole mass spectrometry

目的 为开展农业用水中氨基甲酸酯类农药监测。方法 使用以苯乙烯二乙烯基苯聚合物为填料的ENVI-Chrom P小柱,首次建立针对农田水中15种氨基甲酸酯类农药的固相萃取(SPE)-超高效液相色谱(UPLC)-三重四级杆质谱(QQQ MSD)分析方法。以C_(18)色谱柱为分离柱、甲醇和甲酸水溶液(0. 1%)为流动相、正离子多反应监测(MRM)模式,对前处理和仪器条件进行了优化;并采用上样体积100 ml、以8 ml甲醇进行洗脱,探究了方法的各项特征指标。结果 在1. 00 ng/ml~200 ng/ml浓度内建立内标法标准曲线,所有化合物响应因子的RSD均在10%以内;水样中杂质能有效滤除,且所有化合物方法检出限为0. 004 ng/ml~0. 01 ng/ml;对3个浓度水平的农田水样品分别进行6次平行分析,平均加标回收率为52%~103%,RSD为3. 6%~20. 0%。结论 本研究为控制农田水氨基甲酸酯农药污染奠定了基础。

Objective To monitor carbamate pesticides in agricultural water.Methods A solid phase extraction(SPE)-ultra high performance liquid chromatography(UPLC)-triple quadrupole mass spectrometry(QQQ MSD)method was developed for the first time for the analysis of 15 carbamate pesticides in agricultural water using ENVI-Chrom P column filled with styrene diethylbenzene polymer.C_(18) column was used as separation column,methanol and formic acid aqueous solution(0.1%)were used as mobile phase,and positive ion multiple reaction monitoring(MRM)mode was used to optimize the pretreatment and instrument conditions.The sample volume was 100 ml and 8 ml methanol was used for elution.The characteristic indexes of the method were explored.Results The standard curves of internal standard method were established in the concentration range of 1.00 ng/ml-200 ng/ml,and the RSD of all the response factors were less than 10%.The impurities in water samples can be effectively filtered,and the detection limits of all compounds are 0.004 ng/ml-0.01 ng/ml.The average recoveries and RSDs of water samples were 52%_103%and 3.6%-20.0%,respectively.Conclusion This study laid a foundation for the control of carbamate pesticide pollution in farmland water.