Ege University, Science Faculty, Department of Chemistry, 35100 Bornova, İzmir, Turkey.
Food Chem. 2013 May 1;138(1):54-61. doi: 10.1016/j.foodchem.2012.10.053. Epub 2012 Nov 8.
A gas chromatographic method for the determination of endocrine disruptor pesticides (Chlorpyrifos, Penconazole, Procymidone, Iprodione, Bromopropylate and Lambda-Cyhalothrin) in wine samples is described. A general DFG-S19 method for residual pesticide determination in all kind of food stuff was investigated to simplify and adopt for wine samples in this work. Alternative sample preparation routes were elucidated and compared according to their recovery values. Four different separation techniques were tested and the method employing florosil column after a LLE procedure was applied for wine samples with satisfactory recovery ratios (72-97%). The pesticides were extracted from the sample by cyclohexane-ethyl acetate mixture (1:1 v/v) and cleaned up by florosil column. The regression coefficients were at least 0.99 and relative standard deviations were no higher than 16%. Detection limits were in the range of 0.6-2.9 ng/mL and the relative expanded measurement uncertainties were calculated in the 7-22% range.
本文描述了一种用于测定葡萄酒样品中内分泌干扰农药（毒死蜱、戊唑醇、菌核净、丙环唑、溴丙酰和高效氯氟氰菊酯）的气相色谱方法。本工作研究了一种用于各种食品中残留农药测定的通用 DFG-S19 方法，以简化并适用于葡萄酒样品。根据回收率值，阐明并比较了替代的样品制备路线。测试了四种不同的分离技术，采用 LLE 程序后的氟硅柱方法用于葡萄酒样品，具有令人满意的回收率（72-97%）。通过环己烷-乙酸乙酯混合物（1:1 v/v）从样品中提取农药，并通过氟硅柱进行净化。回归系数至少为 0.99，相对标准偏差不高于 16%。检测限在 0.6-2.9ng/mL 范围内，相对扩展测量不确定度在 7-22%范围内计算。
