杀螟丹中间体硫氰化物及其异构体的高效液相色谱分析

Quantitative Analysis of Intermediate of Cartap and Its by-Product by HPLC

[目的]建立杀螟丹中间体硫氰化物2-N,N-二甲胺基-1,3-二硫氰基丙烷和其异构体1-N,N-二甲胺基-2,3-二硫氰基丙烷的高效液相色谱分析方法。[结果]液相色谱条件：流动相为乙腈-水（体积比50∶50）,流速1.0 mL/min,Sinochrom ODS-BP C18柱,紫外可变波长检测器,检测波长254 nm。外标法对硫氰化物和其异构体进行定量分析,线性相关系数大于0.999,平均回收率分别为103.2%~105.5%和102.4%~106.1%。[结论]该法简便、重复性好、各成分分离良好,可用于杀螟丹中间体的含量分析。

[Aims]The aim is to establish a method for quantitative analysis of intermediate of cartap（N,N-dimethyl-1,3-dithiocyanatopropan-2-amine） and its by-product（N,N-dimethyl-2,3-dithiocyanatopropan-1-amine） by HPLC.[Results] The liquid chromatography condition was as follows： mobile phase was acetonitrile-water（50：50,by vol） on Sinochrom ODS-BP C18 column at a flow rate of 1.0 mL/min,UV detector wavelength was 254 nm and injection volume was 10.0 μL.The quantitative analysis was carried out with the external standard method.The linear correlation coefficient was over 0.999.The detection limit was 5.1-17.4 mg/L.The average recovery ratios for intermediate of cartap and its by-product were 103.2-105.5% and 102.4-106.1% respectively.[Conclusions] The described method was simple with good repeatability and separation and could be used for the quality control of the intermediate of cartap.