REQUIMTE, Instituto Superior de Engenharia, Instituto Politécnico do Porto, Rua Dr° António Bernardino de Almeida, 431, P-4200-072 Porto, Portugal.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2012;29(7):1074-84. doi: 10.1080/19440049.2012.682319. Epub 2012 May 9.
This paper describes a comparison of adaptations of the QuEChERS (quick, easy, cheap, effective, rugged and safe) approach for the determination of 14 organochlorine pesticide (OCP) residues in strawberry jam by concurrent use of gas chromatography (GC) coupled to electron capture detector (ECD) and GC tandem mass spectrometry (GC-MS/MS). Three versions were tested based on the original QuEChERS method. The results were good (overall average of 89% recoveries with 15% RSD) using the ultrasonic bath at five spiked levels. Performance characteristics, such as accuracy, precision, linear range, limits of detection (LOD) and quantification (LOQ), were determined for each pesticide. LOD ranged from 0.8 to 8.9 µg kg(-1); LOQ was in the range of 2.5-29.8 µg kg(-1); and calibration curves were linear (r(2)>0.9970) in the whole range of the explored concentrations (5-100 µg kg(-1)). The LODs of these pesticides were much lower than the maximum residue levels (MRLs) allowed in Europe for strawberries. The method was successfully applied to the quantification of OCP in commercially available jams. The OCPs were detected lower than the LOD.
本文描述了一种改进的 QuEChERS(快速、简单、廉价、有效、耐用和安全)方法,用于同时使用气相色谱(GC)-电子捕获检测器(ECD)和 GC 串联质谱(GC-MS/MS)测定草莓果酱中的 14 种有机氯农药(OCP)残留。根据原始 QuEChERS 方法,测试了三种版本。在五个加标水平下,使用超声浴得到了良好的结果(总体平均回收率为 89%,相对标准偏差为 15%)。对每种农药均进行了准确度、精密度、线性范围、检测限(LOD)和定量限(LOQ)等性能特征的测定。LOD 范围为 0.8-8.9 µg kg(-1);LOQ 范围为 2.5-29.8 µg kg(-1);在探索浓度范围内(5-100 µg kg(-1)),校准曲线均呈线性(r(2)>0.9970)。这些农药的 LOD 远低于欧洲允许的草莓最大残留限量(MRL)。该方法成功应用于市售果酱中 OCP 的定量。OCP 的检测值低于 LOD。