Department of Instrumental Analysis and Environmental Chemistry, IQOG, CSIC, Juan de la Cierva 3, 28006 Madrid, Spain.
J Chromatogr A. 2009 Oct 23;1216(43):7307-13. doi: 10.1016/j.chroma.2009.05.013. Epub 2009 May 15.
The feasibility of a miniaturised generic sample preparation method based on matrix solid-phase dispersion for the determination of three relevant classes of pesticides (organophosphorus pesticides, triazines and pyrethroids) in selected fruits, i.e. orange, apple, pear and grape, have been demonstrated. Satisfactory results were obtained with gas chromatography coupled to mass spectrometry with recoveries of 78-113% in orange, 62-102% in grape, 71-116% in apple and 91-110% in pear, and reproducibilities in general below 20%. The feasibility of simultaneous separation of the three families of pesticides by comprehensive two-dimensional gas chromatography with micro-electro-capture detector was also evaluated. Columns with different polarity and selectivity, including ZB-5, HT-8 and DB-17, were assayed as first dimension and combined with columns of increasing polarity in the second dimension, i.e. HT-8, BPX-50 and Supelcowax-10. The best results for real-life samples after treatment by the proposed miniaturised method were achieved with ZB-5 x BPX-50 column combination. The low limits of detection achieved with this technique (in general, below 0.56 microg/kg) proved its suitability for accurate monitoring of the pesticides classes included in the study at the maximum residue levels set in the European Union.
已经证明了一种基于基质固相分散的微型通用样品制备方法对于确定三种相关类别的农药（有机磷农药、三嗪类和拟除虫菊酯类）在选定水果（即橙、苹果、梨和葡萄）中的可行性。使用气相色谱-质谱联用技术得到了令人满意的结果，在橙中回收率为 78-113%，在葡萄中回收率为 62-102%，在苹果中回收率为 71-116%，在梨中回收率为 91-110%，重现性通常低于 20%。还评估了通过带有微电捕获检测器的全二维气相色谱同时分离这三种农药家族的可行性。使用了具有不同极性和选择性的柱子，包括 ZB-5、HT-8 和 DB-17，作为第一维，并与第二维中极性逐渐增加的柱子（即 HT-8、BPX-50 和 Supelcowax-10）结合。经过提议的微型方法处理后的实际样品，使用 ZB-5 x BPX-50 柱组合获得了最佳结果。该技术实现的低检测限（通常低于 0.56μg/kg）证明其适用于在欧盟设定的最大残留水平下对研究中包含的农药类别进行准确监测。
