REQUIMTE, Instituto Superior de Engenharia do Porto, Porto, Portugal.
J Sep Sci. 2012 Jun;35(12):1521-30. doi: 10.1002/jssc.201200087.
A QuEChERS method has been developed for the determination of 14 organochlorine pesticides in 14 soils from different Portuguese regions with wide range composition. The extracts were analysed by GC-ECD (where GC-ECD is gas chromatography-electron-capture detector) and confirmed by GC-MS/MS (where MS/MS is tandem mass spectrometry). The organic matter content is a key factor in the process efficiency. An optimization was carried out according to soils organic carbon level, divided in two groups: HS (organic carbon >2.3%) and LS (organic carbon <2.3%). The method was validated through linearity, recovery, precision and accuracy studies. The quantification was carried out using a matrix-matched calibration to minimize the existence of the matrix effect. Acceptable recoveries were obtained (70-120%) with a relative standard deviation of ≤16% for the three levels of contamination. The ranges of the limits of detection and of the limits of quantification in soils HS were from 3.42 to 23.77 μg kg(-1) and from 11.41 to 79.23 μg kg(-1), respectively. For LS soils, the limits of detection ranged from 6.11 to 14.78 μg kg(-1) and the limits of quantification from 20.37 to 49.27 μg kg(-1) . In the 14 collected soil samples only one showed a residue of dieldrin (45.36 μg kg(-1) ) above the limit of quantification. This methodology combines the advantages of QuEChERS, GC-ECD detection and GC-MS/MS confirmation producing a very rapid, sensitive and reliable procedure which can be applied in routine analytical laboratories.
建立了一种 QuEChERS 方法,用于测定来自葡萄牙不同地区的 14 种土壤中 14 种有机氯农药的含量,这些土壤的组成范围很广。采用气相色谱-电子捕获检测(GC-ECD)对提取物进行分析,并通过气相色谱-串联质谱(GC-MS/MS)进行确认。有机质含量是影响过程效率的关键因素。根据土壤有机碳水平进行了优化,分为 HS(有机碳>2.3%)和 LS(有机碳<2.3%)两组。通过线性、回收率、精密度和准确度研究对方法进行了验证。采用基质匹配校准进行定量,以最大程度地减少基质效应的存在。在三种污染水平下,回收率均在 70-120%之间,相对标准偏差≤16%。HS 土壤中检测限和定量限的范围分别为 3.42-23.77μg/kg 和 11.41-79.23μg/kg。对于 LS 土壤,检测限的范围为 6.11-14.78μg/kg,定量限的范围为 20.37-49.27μg/kg。在所采集的 14 个土壤样本中,只有一个样本中的狄氏剂残留量(45.36μg/kg)超过了定量限。该方法结合了 QuEChERS、GC-ECD 检测和 GC-MS/MS 确证的优点,具有快速、灵敏、可靠的特点,可应用于常规分析实验室。