Mundy D E, Machin A F
J Chromatogr. 1981 Oct 30;216:229-38. doi: 10.1016/s0021-9673(00)82351-1.
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.
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。