毛细管气相色谱法测定阿仑膦酸钠原料药中甲烷磺酸乙酯的残留量

Determination of Residual Ethyl Methyl Sulfonate in Alendronate Sodium by GC

目的：建立测定阿仑膦酸钠原料药中甲烷磺酸乙酯残留量的方法。方法：采用毛细管气相色谱法。色谱柱为HP．5毛细管色谱柱，载气为氮气，柱温为100℃保持8min，流速为1．0ml／min，进样量为1．0μl，分流比为10：1，进样口温度为220℃，检测器为氢火焰离子化检测器．检测器温度为300℃。结果：甲烷磺酸乙酯检测质量浓度在3．92～27．44μg／ml范围内与峰面积积分值呈良好的线性关系（r=0．9997）；精密度、稳定性、重复性试验的RSD≤2．30％；平均回收率为97．94％，RSD：1．48％（n=9）。3批样品中均未检出甲烷磺酸乙酯。结论：该方法简便、灵敏、可靠，可用于阿仑膦酸钠原料药中甲烷磺酸乙酯残留量的测定。

OBJECTIVE： To establish the method for the determination of residual ethyl methyl sulfonate in alendronate sodium raw material. METHODS： Capillary GC method was adopted. The determination was performed on HP-5 capillary column with ni- trogen as carrier gas at the flow rate of 1.0 ml/min. The column temperature was 100 ℃ for 8 min, and sample size was 1.0 μl. The split ratio was 10 ： 1, and temperature of injector was 220 ℃. The flame ionization detector was used with the temperature of 300 ℃. RESULTS： The linear range of ethyl methyl sulfonate were 3.92-27.44μg/ml （r=0.999 7） with average recovery of 97.94% （RSD= 1.48%, n=9）. RSDs of precision, stability and reproducibility tests were all lower than 2.30%. Ethyl methyl sul- fonate was not detected in 3 batches of samples. CONCLUSIONS： The established method is simple, sensitive and reliable, and it can be used for the content determination of ethyl methyl sulfonate in alendronate sodium.