Sawyer L D
J Assoc Off Anal Chem. 1982 Sep;65(5):1122-8.
A combined sample preparation/extraction procedure is presented for pesticide residue analysis of oilseeds and related high fat-low moisture products. The procedure utilizes high-speed milling to prepare the sample and high-speed homogenization in the extraction step to achieve what is apparently quantitative isolation of both incurred residues and natural oils. A separate, simple, oil determination step allows findings to be reported on either the fat or whole product basis. Petroleum ether, ethyl ether-petroleum ether (1 + 1), and ethanol are used serially as the extractants. Usual fatty food cleanup procedures and multiresidue gas chromatographic detection techniques are utilized. The procedure presented in this paper is a refinement of earlier work which used a homogenizer both to grind and to extract samples of unground seeds and which demonstrated essentially complete extraction of endrin residues in soybeans and DDT residues in mustard seed. Identical samples analyzed by the currently recommended shakeout procedure, 29.012, gave recoveries of approximately 50% of the total residues. The procedure presented in this paper was satisfactorily tested on 13 different oilseed types and one sample of soda crackers. Oil content for these samples ranged from 5 to 69%.
本文介绍了一种用于油籽及相关高脂肪低水分产品农药残留分析的联合样品制备/提取方法。该方法在样品制备步骤中采用高速研磨，在提取步骤中采用高速匀浆，以实现对所含残留农药和天然油脂的明显定量分离。一个单独的、简单的油脂测定步骤使得检测结果可以基于脂肪或整个产品进行报告。依次使用石油醚、乙醚 - 石油醚（1 + 1）和乙醇作为萃取剂。采用常规的高脂肪食品净化程序和多残留气相色谱检测技术。本文所介绍的方法是对早期工作的改进，早期工作使用匀浆器研磨并提取未研磨种子的样品，且证明了在大豆中狄氏剂残留和芥菜种子中滴滴涕残留的基本完全提取。采用当前推荐的振荡提取程序29.012对相同样品进行分析，总残留回收率约为50%。本文介绍的方法在13种不同油籽类型和一个苏打饼干样品上进行了令人满意的测试。这些样品的含油率在5%至69%之间。
