高效液相色谱法测定杀线威的含量

Determination of oxamyl by HPLC

目的建立测定杀线威的高效液相色谱法。方法采用C18色谱柱,以甲醇—水(85∶15)为流动相,流速0.8 ml/min,检测波长234 nm,选用灭多威为内标物,内标法测定杀线威原料药的含量。结果在杀线威浓度为2μg/ml^80μg/ml范围内,杀线威色谱峰面积(AS)和内标灭多威色谱峰面积(AM)的比值(RS/M)与杀线威的浓度(C)呈良好的线性关系,线性方程为:RS/M=6.53×10-2C+4.91×10-3,r=0.999 8(n=6),待测样品杀线威与内标物的色谱峰分离完全,二者分离度R>1.5,高、中、低三种浓度的加样回收率100.2%、99.12%、98.82%,日内精密度(RSD)小于0.67%。结论该方法灵敏、快速,操作简便,测定结果准确可靠。

Objective： To determine the contents of oxamyl by HPLC. Methods： The liquid chromatography was carfled out by the use of Waters symmetry shieldTM RP18 column （150 mm 3.9 mm, 5 μm） with the detection wavelength at 234 nm.The flowrate of mobile phase （methanol-water, 85：15） was 0.8 ml. min^-1 and the internal standard was methmyl oxime. Results; There was a good linear relationship within the range of 2- 80μg·ml^- 1 （ r= 0. 9998, n = 6）. The average recovery was 98.82 % - 100.2 %, and RSD in the day was 0.67 %. Conclusion： The method is simple, rapid, selective and sensitive.