Pesticide Chemistry and Toxicology Laboratory, Department of Agricultural Biotechnology and Research Institute of Agriculture and Life Sciences, Seoul National University, Seoul, 08826, South Korea.
Drug Metabolism and Bioanalysis Laboratory, College of Pharmacy, The Catholic University of Korea, Bucheon, 14662, Republic of Korea.
Chemosphere. 2021 Aug;277:130215. doi: 10.1016/j.chemosphere.2021.130215. Epub 2021 Mar 15.
Multiresidual pesticide analysis in hair can provide useful perspectives on the relationship between pesticides and human health. To establish a rapid and simultaneous analytical method using LC-MS/MS and GC-MS/MS, optimization of hair pulverization, extraction solvent and purification with dispersive SPE was performed for 300 pesticides. Hair pulverization was standardized with a ball mill, at 30 Hz for 20 min (10 min twice), using 3-mm diameter beads. For extraction, 0.1% formic acid in acetonitrile was selected, and PSA d-SPE was chosen for clean-up among three different types of solid phase extraction. The limits of quantitation (LOQs) in this method were between 2.5 and 7.5 pg mg. In recovery test, fifty milligrams of hair powder were extracted with 0.1% formic acid in acetonitrile, and incubated for three h at 40 ℃. The crude extract was treated using PSA-dSPE, dried under nitrogen gas, and reconstructed with acetonitrile. An aliquot was analyzed with LC- and GC-MS/MS. Recovery ranges were 22.7-131.1%, in LC-MS/MS analysis, and 81.1-151.8% in GC-MS/MS analysis. The validated analysis systems were applied to biomonitoring of ten agricultural workers, and residues of 28 target pesticides were detected in their hair.
多残留农药分析在头发中可以提供关于农药与人类健康之间关系的有用视角。为了建立一种使用 LC-MS/MS 和 GC-MS/MS 的快速同时分析方法，对头发粉碎、提取溶剂和分散固相萃取净化进行了优化，以分析 300 种农药。头发粉碎采用球磨机标准化，以 30 Hz 粉碎 20 分钟（10 分钟两次），使用 3 毫米直径的珠子。对于提取，选择 0.1%甲酸在乙腈中，在三种不同类型的固相萃取中选择 PSA d-SPE 进行净化。该方法的定量限 (LOQ) 在 2.5 至 7.5 pg mg 之间。在回收测试中，将 50 毫克头发粉末用 0.1%甲酸在乙腈中提取，并在 40℃下孵育 3 小时。粗提物用 PSA-dSPE 处理，氮气干燥，用乙腈重建。取一份进行 LC-MS/MS 和 GC-MS/MS 分析。LC-MS/MS 分析的回收率范围为 22.7-131.1%，GC-MS/MS 分析的回收率范围为 81.1-151.8%。验证后的分析系统应用于 10 名农业工人的生物监测，在他们的头发中检测到 28 种目标农药的残留。
