气相色谱法测定注射用去水卫矛醇的含量及有关物质

Determination of Dianhydrogalactitol for Injection and Related Substances by GC

目的:建立注射用卫矛醇含量及有关物质的气相色谱法。方法:采用Agilent DB-1(30 m×0.53 mm,1.5μm);程序升温:起始温度为100℃,维持3 min,以10℃·min^(-1)升至200℃,维持5 min;进样口温度为250℃,检测器F1D温度为250℃;载气为氮气,流速为5 ml·min^(-1)。结果:去水卫矛醇与其相邻杂质峰能完全分离,去水卫矛醇在0.010 05～1.005 mg·ml^(-1)浓度范围内线性关系良好(r=0.999 1),平均回收率为101.1%(RSD=1.12%,n=9)。结论:本方法操作简单,精密度好,结果准确可靠,可用于该制剂的质量控制。

Objective： To establish a GC method for determination of assay and related substances of dianhydrogalaetitol for injection. Method： Using a GC method with a capillary column, which temperature rose by program. The initial temperature was 100 ℃ , maintained for 3 rain, raised to 200 ℃ with a rate of 10 ℃ · min^- 1, then maintained for 5 min. The temperature of injection port was 250 ℃ and the temperature of FID detection was 250 ℃. The carrier gas was nitrogen and the flow rate was 5 ml. min^-1. Result： The data showed that this method could clearly separate dianhydrogalactitol peak from its nearby impurity peaks, with a better linear range of 0. 010 05-1. 005 mg· ml^- 1 （r = 0. 999 1 ） , and the average recovery range of 101.1% （RSD = 1.12% , n = 9 ）. Conclusion： This method is simple, accurate and liable,it can be used for quality control of this preparation.