盐酸倍他司汀中基因毒性杂质甲醛的测定

Determination of genotoxic impurity formaldehyde in betahistine hydrochloride

目的建立气相色谱法测定盐酸倍他司汀原料中甲醛的含量。方法采用6%氰丙基苯基-94%二甲基聚硅氧烷为固定液的毛细管柱(30 m×0.25 mm,0.25μm),溶液直接进样,以水为溶剂,程序升温,氢火焰离子化检测器,进样口温度为230℃,检测器温度为250℃。结果溶剂不干扰测定。甲醛在0.055~1.109 ng·mL^(-1)与测定值线性良好,重复性良好,检测限为0.018 ng·mL^(-1),定量限为0.055 ng·mL^(-1),低、中、高浓度甲醛的平均回收率分别为100.6%、96.9%、97.0%,RSD分别为0.79%、2.1%、1.9%。结论该方法简便、准确、灵敏度高、重现性好,适用于盐酸倍他司汀中基因毒性杂质甲醛的检查。

Objective To determine formaldahyde in betahistine hydrochloride by gas chromatography method.Methods Formaldahyde was separated on a DB-624 capillary chromatographic column (30m×0.25 mm,0.25μm) with temperature programming.Nitrogen was used as the carrier gas.The temperature of the injector was 230℃.The temperature of flame ionization detector was 250℃.Results Determination was not interferred by the solvent.Good linearity was showed in the range of0.055-1.109 ng·mL^(-1).The LOD and LOQ of formaldahyde in betahistine hydrochloride was 0.018ng·mL^(-1)and 0.055 ng·mL^(-1),respectively.The average recovery rate of low,medium and high dose formaldahyde was 100.6%,96.9%,and 97.0%with RSD at 0.79%,2.1%and 1.9%,respectively.Conclusion The method is specific,accurate and convenient,which can be used for the determination of formaldahyde in betahistine hydrochloride.