Instituto Murciano de Investigación y Desarrollo Agrario y Alimentario, IMIDA, C/Mayor s/n, La Alberca, 30150 Murcia, Spain.
Talanta. 2011 Aug 15;85(2):975-82. doi: 10.1016/j.talanta.2011.05.012. Epub 2011 May 12.
In this work, a rapid and sensitive analytical multiresidue method has been developed for the simultaneous determination of 48 pesticides and 19 metabolites in waters (tap, leaching and sewage), using liquid chromatography-tandem mass spectrometry (LC-MS/MS) with triple quadrupole in selected reaction monitoring (SRM) mode. The procedure involves initial single phase extraction of samples with acetonitrile by sonication, followed by liquid-liquid partition aided by "salting out" process using NaCl. Matrix influence on recoveries was evaluated for the three waters. More than 50% of the compound presented very low signal suppression. The method presents good linearity over the range assayed 10-500 μg L(-1) and the most frequent detection limits was 0.05 ng mL(-1). The average recovery by the LC-MS/MS method obtained for these compounds varied from 74.6 to 111.2% with a relative standard deviation between 2.5 and 8.9%. The proposed method was used to determine pesticides levels in leaching water samples from 5 lysimeters from an experimental greenhouse located in Murcia.
在这项工作中,开发了一种快速灵敏的分析多残留方法,用于同时测定水中(自来水、淋溶水和污水)的 48 种农药和 19 种代谢物,使用液相色谱-串联质谱(LC-MS/MS),采用三重四极杆在选择反应监测(SRM)模式下进行分析。该方法包括首先用乙腈对样品进行超声单阶段提取,然后通过"盐析"过程进行液-液分配。对三种水样进行了基质对回收率的影响评估。超过 50%的化合物表现出非常低的信号抑制。该方法在测定范围内具有良好的线性关系,范围为 10-500μg/L,最常见的检测限为 0.05ng/mL。通过 LC-MS/MS 方法获得的这些化合物的平均回收率为 74.6%至 111.2%,相对标准偏差在 2.5%至 8.9%之间。该方法用于测定位于穆尔西亚的一个实验温室的 5 个淋溶仪中淋溶水样中的农药水平。