Muir D C, Grift N P
J Assoc Off Anal Chem. 1983 May;66(3):684-90.
Methods for determination of triaryl/alkylphosphates (TAPs) in water, fish, and sediment have been extended to determination of the diarylphosphate (DAP) degradation products. DAPs were extracted from water (adjusted to pH 0.5) by use of XAD-2 resin and determined by gas-liquid chromatography as butyl esters. Recovery of diphenylphosphate (DPP) and o-, m-, p-dicresylphosphates (DoCP, DmCP, DpCP) were greater than 95% in water samples fortified at 1, 10, and 50 micrograms/L. DAPs were extracted from fish with methanol and the extracts were cleaned up on reverse phase (C18) silica cartridges. Recoveries were greater than 87% for DPP, DoCP, DmCP, and DpCP in fish muscle fortified at 50, 100, and 500 ng/g. Sediments were refluxed with aqueous methanol and DAPs were recovered by use of XAD-2 resin. Recoveries of DAPs from sediments fortified at 50 and 100 ng/g were greater than 76%. Interferences (1-10 ng/g) from phosphorus or nitrogen-containing GLC peaks prevented sub- ng/g level analysis for DAPs in sediment and fish extracts.
测定水、鱼类和沉积物中三芳基/烷基磷酸酯（TAPs）的方法已扩展至测定二芳基磷酸酯（DAP）降解产物。通过使用XAD - 2树脂从水（调节至pH 0.5）中提取DAPs，并通过气液色谱法将其测定为丁酯。在添加浓度为1、10和50微克/升的水样中，磷酸二苯酯（DPP）以及邻、间、对二甲基苯基磷酸酯（DoCP、DmCP、DpCP）的回收率大于95%。用甲醇从鱼类中提取DAPs，提取物在反相（C18）硅胶柱上进行净化处理。在添加浓度为50、100和500纳克/克的鱼肉中，DPP、DoCP、DmCP和DpCP的回收率大于87%。沉积物与甲醇水溶液回流，通过使用XAD - 2树脂回收DAPs。在添加浓度为50和100纳克/克的沉积物中，DAPs的回收率大于76%。来自含磷或含氮气相色谱峰的干扰（1 - 10纳克/克）妨碍了对沉积物和鱼类提取物中DAPs进行低于纳克/克水平的分析。
