顶空气相色谱法测定唑来膦酸中有机溶剂残留量

Determination of Residual Solvent in Zoledronic Acid by Headspace GC

目的采用顶空气相色谱法测唑来膦酸中有机溶剂残留量。方法用DB-624毛细管柱(30 m×0.32 mm,1.8μm),柱温为起始温度40℃,维持10 min,再以每分钟35℃的速率升温至220℃,维持5 min;进样口温度为250℃;氢火焰离子化检测器(FID);检测器温度为280℃。结果6种溶剂的分离度良好,在所考察的质量浓度范围内线性关系良好,r=0.999 9,平均回收率为96.9%~102.3%,检出限为7.86 pg/mL^75.0 ng/mL。结论所用方法简单、灵敏度高,可用于唑来膦酸中有机溶剂残留量的限度检查。

Objective To adopt the headspace gas chromatography（GC） method for determining the residual solvent in zoledronic acid. Methods The DB-624 capillary column（30 m×0. 32 mm, 1.8 μm） was adopted;the initial temperature was 40℃ ,maintained for 10 min,then heated up to 220 ~C with the rate of 30 ℃/min and maintained for 5min at 220 ℃ ;the injector port temperature was 250 ℃; the FID detector temperature was at 280 ~C. Results Several solvents of methanol, ethanol, acetone, acetonitrile, dichloromethane and hexane had the good separation degrees and good linear relations during the investigated concentration range, r = 0. 999 9 ,the aver- age recovery rate was 96.9%-102.3%.The detection limit was 7.86-75.0 ng/mL. Conclusion The used method is simple with high sensitivity and can be applied to the limit test of residual organic solvent in zoledronic acid.