Dale W E, Miles J W, Churchill F C
J Assoc Off Anal Chem. 1976 Sep;59(5):1088-93.
A gas-liquid chromatographic method has been developed for the analysis of residues of chlorphoxim, 2-chloro-alpha ((diethoxyphosphinothioyl)oxy)imino)-benzeneacetonitrile, in water and fish. The method is based on the in-block methylation of chlorphoxim with 0.01M trimethylanilinium hydroxide in methanol. The derivative, O,O-diethyl O-methyl phosphorothioate, was determined quantitatively by using a flame photometric detector specific for phosphorus. The in-block reaction is 70% efficient. Water samples were extracted with hexane; fish were extracted with methylene chloride and cleaned up on an acetonitrile-hexane partition column. Recoveries from water and fish samples spiked with chlorphoxim averaged 86.3 and 80.4%, respectively. Limits of detection were 10.0 ppb for 5 g samples of fish and 0.10 ppb for 300 ml water samples.
已开发出一种气相色谱法，用于分析水中和鱼类中氯辛硫磷（2-氯-α-（二乙氧基磷酰硫基）氧基）亚氨基苯乙腈）的残留量。该方法基于氯辛硫磷在甲醇中与0.01M氢氧化三甲基苯胺进行的分子内甲基化反应。衍生物O，O-二乙基O-甲基硫代磷酸酯通过使用对磷具有特异性的火焰光度检测器进行定量测定。分子内反应的效率为70%。水样用己烷萃取；鱼样用二氯甲烷萃取，并在乙腈-己烷分配柱上进行净化。添加氯辛硫磷的水和鱼样的回收率平均分别为86.3%和80.4%。5g鱼样的检测限为10.0ppb，300ml水样为0.10ppb。
