González-Curbelo Miguel Á, Dionis-Delgado Samara, Asensio-Ramos María, Hernández-Borges Javier
Departamento de Química Analítica, Nutrición y Bromatología, Facultad de Química, Universidad de La Laguna (ULL), La Laguna, Tenerife, Spain.
J Sep Sci. 2012 Jan;35(2):299-307. doi: 10.1002/jssc.201100811.
Analytical potentiality of a modified version of the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method has been studied and validated for the extraction of a group of 11 pesticides (ethoprophos, cadusafos, dimethoate, terbufos, disulfoton, chlorpyrifos-methyl, fenitrothion, pirimiphos-methyl, malathion, chlorpyrifos and fensulfothion) and some of their metabolites (malaoxon, disulfoton sulfoxide, terbufos sulfone and disulfoton sulfone) in toasted barley and chickpea flours. The method involves separation and quantification by gas chromatography (GC) with nitrogen phosphorus detection (NPD) using triphenylphosphate as the internal standard. Matrix-matched calibration was carried out for both flours due to the existence of a matrix effect. Linearity, recovery, precision and accuracy studies of the proposed QuEChERS-GC-NPD method were evaluated in each sample matrix. Mean recovery values were in the range of 73-118% with relative standard deviation values below 10%. Limits of detection of the whole method were between 0.07 and 57.39 μg/kg. The method was finally applied for the analysis of 14 samples collected in different zones of the Tenerife island. The residues of pirimiphos-methyl were found in 13 of them, confirming its unequivocal presence by mass spectrometry.
已对改良版的QuEChERS（快速、简便、廉价、高效、耐用且安全）方法的分析潜力进行了研究，并验证了该方法用于提取烤大麦粉和鹰嘴豆粉中一组11种农药（丙线磷、硫线磷、乐果、特丁硫磷、乙拌磷、甲基毒死蜱、杀螟硫磷、甲基嘧啶磷、马拉硫磷、毒死蜱和丰索磷）及其一些代谢物（马拉氧磷、乙拌磷亚砜、特丁硫磷砜和乙拌磷砜）的效果。该方法包括使用磷酸三苯酯作为内标，通过带氮磷检测（NPD）的气相色谱（GC）进行分离和定量。由于存在基质效应，对两种面粉均进行了基质匹配校准。在所提出的QuEChERS-GC-NPD方法中，对每个样品基质进行了线性、回收率、精密度和准确度研究。平均回收率值在73%-118%范围内，相对标准偏差值低于10%。整个方法的检测限在0.07至57.39μg/kg之间。该方法最终应用于分析从特内里费岛不同区域采集的14个样品。其中13个样品中检测到甲基嘧啶磷残留，通过质谱法确认了其明确存在。
