薄层色谱-光度法测定亚胺硫磷中O,O-二甲基-S-(邻苯二甲酰亚胺基甲基)二硫代磷酸酯

Determination of O,O-dimethyl-S(3phthalimidomethyl) phosphorodithio-ate in phesmet by photometry hyphenated with thin layer chromatography

目的：建立薄层色谱-光度法测定亚胺硫磷中O,O-二甲基-S-（邻苯二甲酰亚胺基甲基）二硫代磷酸酯的方法。方法：采用薄层层析分离样品中的干扰物质,用乙醇淋洗,浓缩后,经浓硝酸-高氯酸硝化,加热分解,用磷钼酸铵显色,光度法测定样品中O,O-二甲基-S-（邻苯二甲酰亚胺基甲基）二硫代磷酸酯。结果：该方法的线性范围0~100μg/50 ml,相关系数为0.9995,样品加标回收率95%~100%。结论：本法操作简单、快速、结果准确可靠,应用于实际样品的测定,结果满意。

Objective： To establish a method for detection of O, O - dimethyl - S - （phthalimidomethyl） - phosphorodithioate in phesmet. Methods：The method of thin layer chromatograpty （TLC） was used to separate the main component, chromatographic band of the sample which contains the phesmet taken down from the TCL plate. Then the sample was digested with nitric acid - perchloric acid. The removing was taken up with HNO3 and the PO4^3- transformed from phesmet and determined photometricalh. Results：The calibration curve for O, O -dimethyl -S - （phthalimidomethyl） -phosphorodithioate in phesmet was 0 - 100 ug/50 ml, r =0. 9995, and the recovery of standard addition 95% to 100%. Conclusion：This method is simple, rapid, sensitive and of accurate results. The method has been applied to the sample analysis with satisfactory results.