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高效液相色谱法和气相色谱法测定动物材料中的五氯苯酚及相关化合物

Determination of pentachlorophenol and related compounds in animal materials by high-performance liquid chromatography and gas chromatography.

作者信息

Mundy D E, Machin A F

出版信息

J Chromatogr. 1981 Oct 30;216:229-38. doi: 10.1016/s0021-9673(00)82351-1.

Abstract

The rapid determination of pentachlorophenol and tetrachlorophenols in animal materials by high-performance liquid chromatography (HPLC) on porous silica is described. Non-fatty substrates are digested in alkali and the chlorophenols extracted as ion pairs. Fatty materials are extracted with ethyl acetate-hexane after acidification. Extracts are cleaned up on "Sep-Pak" silica or Florisil cartridges. Penta- and tetrachloroanisoles are recovered by the extraction procedures and can be determined by gas chromatography if required. Mean recoveries of the chlorophenols were 73-108% at fortification levels of 0.1-10 mg/kg. A concentration of 0.1 mg/kg can readily be determined and the method can be adapted to reach about 1 microgram/kg. Identities can be confirmed by ion-pair HPLC on a reversed-phase column.

摘要

本文描述了采用高效液相色谱法(HPLC)在多孔硅胶上快速测定动物材料中五氯苯酚和四氯苯酚的方法。非脂肪性底物在碱性条件下消化,氯酚以离子对形式萃取。脂肪性材料在酸化后用乙酸乙酯 - 己烷萃取。萃取液在“Sep - Pak”硅胶或弗罗里硅土柱上进行净化处理。五氯苯甲醚和四氯苯甲醚可通过萃取程序回收,如有需要可通过气相色谱法测定。在添加水平为0.1 - 10 mg/kg时,氯酚的平均回收率为73 - 108%。0.1 mg/kg的浓度很容易测定,该方法经调整后可达到约1微克/千克的检测限。可通过反相柱上的离子对HPLC法确认其身份。

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