Feng Xue, He Zeying, Wang Lu, Peng Yi, Luo Ming, Liu Xiaowei
Ministry of Agriculture, Agro-Environmental Protection Institute, Tianjin, P.R. China.
College of Food Science and Technology, Henan Agricultural University, Zhengzhou, P.R. China.
J Sep Sci. 2015 Sep;38(17):3047-54. doi: 10.1002/jssc.201500412. Epub 2015 Jul 16.
A new method for simultaneous determination of 36 pesticides, including 15 organophosphorus, six carbamate, and some other pesticides in soil was developed by liquid chromatography with tandem quadruple linear ion trap mass spectrometry. The extraction and clean-up steps were optimized based on the quick, easy, cheap, effective, rugged, and safe method. The data were acquired in multiple reaction monitoring mode combined with enhanced product ion to increase confidence of the analytical results. Validation experiments were performed in soil samples. The average recoveries of pesticides at four spiking levels (1, 5, 50, and 100 μg/kg) ranged from 63 to 126% with relative standard deviation below 20%. The limits of detection of pesticides were 0.04-0.8 μg/kg, and the limits of quantification were 0.1-2.6 μg/kg. The correlation coefficients (r(2) ) were higher than 0.990 in the linearity range of 0.5-200 μg/L for most of the pesticides. The method allowed for the analysis of the target pesticides in the lower μg/kg concentration range. The optimized method was then applied to the test of real soil samples obtained from several areas in China, confirming the feasibility of the method.
建立了一种采用液相色谱-串联四极杆线性离子阱质谱同时测定土壤中36种农药(包括15种有机磷农药、6种氨基甲酸酯类农药及其他一些农药)的新方法。基于快速、简便、廉价、高效、耐用和安全的方法对萃取和净化步骤进行了优化。数据采集采用多反应监测模式并结合增强产物离子,以提高分析结果的可信度。在土壤样品中进行了验证实验。4个加标水平(1、5、50和100 μg/kg)下农药的平均回收率为63%至126%,相对标准偏差低于20%。农药的检测限为0.04 - 0.8 μg/kg,定量限为0.1 - 2.6 μg/kg。大多数农药在0.5 - 200 μg/L线性范围内的相关系数(r(2))高于0.990。该方法能够分析低至μg/kg浓度范围内的目标农药。然后将优化后的方法应用于从中国多个地区采集的实际土壤样品的检测,证实了该方法的可行性。