Office of Pesticide Programs, Biological and Economic Analysis Division, Analytical Chemistry Branch, US Environmental Protection Agency, 701 Mapes Road, Fort George G Meade, Maryland 20755-5350, USA.
J Agric Food Chem. 2010 May 26;58(10):5862-7. doi: 10.1021/jf9038524.
A rapid multiresidue method that captures residues of the insecticide formetanate hydrochloride (FHCl) in selected fruits is described. The method was used to provide residue data for dietary exposure determinations of FHCl. Using an acetonitrile extraction with a dispersive cleanup based on AOAC International method 2007.01, also known as QuEChERS, which was further modified and streamlined, thousands of samples were successfully analyzed for FHCl residues. FHCl levels were determined both by liquid chromatography-single-stage mass spectrometry (LC-MS) and ultraperformance liquid chromatography (UPLC)-tandem mass spectrometry (LC-MS/MS). The target limit of detection (LOD) and the limit of quantitation (LOQ) achieved for FHCl were 3.33 and 10 ng/g, respectively, with LC-MS and 0.1 and 0.3 ng/g, respectively, with LC-MS/MS. Recoveries at these previously unpublished levels ranged from 95 to 109%. A set of 20-40 samples can be prepared in one working day by two chemists.
一种快速多残留方法,可提取选定水果中杀虫剂(formetanate hydrochloride,FHCl)的残留。该方法用于提供 FHCl 的膳食暴露测定的残留数据。使用乙腈提取,基于 AOAC 国际方法 2007.01(也称为 QuEChERS)的分散净化,进一步进行了修改和简化,数千个样本成功地分析了 FHCl 残留。通过液相色谱-单级质谱 (LC-MS) 和超高效液相色谱 (UPLC)-串联质谱 (LC-MS/MS) 测定 FHCl 水平。LC-MS 和 LC-MS/MS 的 FHCl 目标检测限 (LOD) 和定量限 (LOQ) 分别为 3.33 和 10 ng/g 和 0.1 和 0.3 ng/g。在这些未发表的水平上,回收率范围为 95%至 109%。两名化学家可以在一个工作日内制备 20-40 个样本。