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用于测定禽蛋中三氯杀螨醇的联合萃取-净化柱色谱法。

Combined extraction-cleanup column chromatographic procedure for determination of dicofol in avian eggs.

作者信息

Krynitsky A J, Stafford C J, Wiemeyer S N

机构信息

U.S. Fish and Wildlife Service, Patuxent Wildlife Research Center, Laurel, MD 20708.

出版信息

J Assoc Off Anal Chem. 1988 May-Jun;71(3):539-42.

PMID:3391958
Abstract

Dicofol in avian eggs was completely oxidized to dichlorobenzophenone (DCBP) when a hexane Soxhlet extraction procedure was used. This degradation did not occur with other avian tissues (muscle and liver). For this reason, a combined extraction-cleanup column chromatographic procedure, without added heat, was developed for the determination of dicofol in avian eggs. Homogenized subsamples of eggs were mixed with sodium sulfate, and the mixture was added as the top layer on a column prepacked with Florisil. The dicofol and other compounds of interest were then eluted with ethyl ether-hexane. The extracts, relatively free from lipids, were quantitated on a gas chromatograph equipped with a 63Ni electron-capture detector and a methyl silicone capillary column. Recoveries from chicken eggs, fortified with dicofol and other DDT-related compounds, averaged 96%. Analysis of eggs of eastern screech-owls, fed a meat diet containing 10 ppm technical Kelthane, showed that both dicofol and DCBP were present. Results were confirmed by gas chromatography/mass spectrometry. This method is rapid and reliable, involves a minimum of sample handling, and is well suited for high volume determination of dicofol in eggs and other avian tissues.

摘要

当采用正己烷索氏提取法时,禽蛋中的三氯杀螨醇会完全氧化为二氯二苯甲酮(DCBP)。而其他禽组织(肌肉和肝脏)中不会发生这种降解。因此,开发了一种无需加热的联合提取-净化柱色谱法,用于测定禽蛋中的三氯杀螨醇。将匀浆后的禽蛋子样本与硫酸钠混合,然后将混合物作为顶层添加到预先填充有弗罗里硅土的柱上。接着用乙醚-正己烷洗脱三氯杀螨醇和其他相关化合物。提取物中脂质含量相对较低,在配备有63Ni电子捕获检测器和甲基硅氧烷毛细管柱的气相色谱仪上进行定量分析。向鸡蛋中添加三氯杀螨醇和其他与滴滴涕相关的化合物后进行回收率测定,平均回收率为96%。对喂食含有10 ppm工业用开乐散的肉类食物的东部鸣角鸮的蛋进行分析,结果表明蛋中同时存在三氯杀螨醇和二氯二苯甲酮。结果通过气相色谱/质谱法得到证实。该方法快速可靠,样品处理量最少,非常适合大量测定禽蛋和其他禽组织中的三氯杀螨醇。

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