GC法测定托吡司特中的水合肼残留量

Determination of the Residual Hydrazine Hydrate in Topiroxostat by GC

建立一种气相色谱分析方法,测定托吡司特中的水合肼含量。采用DB-624毛细管色谱柱(30m×0.32mm,5μm);进样口温度为200℃;FID检测器,温度为250℃;升温程序:起始温度为95℃,保持5 min,再以10℃/min的速率升温至180℃,保持0 min,再以30℃/min的速率升温至225℃,保持4 min;载气为高纯氮气;进样量为1μL。结果显示二丙酮腙线性范围为0.00257~0.05135 mg·mL^(-1)(r=1.000);二丙酮腙平均回收率为101.4%,RSD为0.8%。该方法操作简便、快速准确,重复性好。

The gas chromatography(GC)method was established to determine residual hydrazine hydrate in topiroxostat.The determination was performed on DB-624 capillary column(30 m×0.32 mm,5μm)under the programmed temperature.FID was used,the inlet temperature was 200℃ and the detector temperature was 250℃.The high pure nitrogen was used as the carrier gas.The column temperature programmer was set as:remain the starting temperature of 95℃ for 5 min,increase to 180℃ at the rate of 10℃·min^(-1),then increase to 225℃ at the rate of 30℃·min^(-1) and remain 225℃ for 4 min.The injection volume was 1μL.The liner range of acetone azine was 0.00257~0.05135 mg·mL^(-1)(r=1.000).The average recovery rate of acetone azine(n=9)was 101.4%with its RSD value of 0.8%.The method is simple,fast and accurate,and has good repeatability.