顶空气相色谱法测定盐酸左西替利嗪原料药中N,N-二异丙基乙胺残留量

目的:建立盐酸左西替利嗪原料药中N,N-二异丙基乙胺残留量的测定方法。方法:采用顶空气相色谱法,色谱柱为DB-624毛细管柱,顶空进样,顶空瓶加热温度为90℃,加热时间为15 min;程序升温,以氮气为载气,氢火焰离子化检测器温度为250℃。结果:N,N-二异丙基乙胺检测质量浓度线性范围为2.01¹5.08μg/ml(r=0.999 3),总平均回收率为98.81%,RSD为1.34%(n=3),定量限、检测限为0.201、0.101μg/ml。3批样品中N,N-二异丙基乙胺残留量分别为0.006 9%、0.008 8%、0.006 3%。结论:建立的方法快速、灵敏、准确,可用于盐酸左西替利嗪原料药中N,N-二异丙基乙胺残留量的测定。

Determination of Residual N,N-Diisopropylethylamine in Levocetirizine Hydrochloride Raw Material by Headspace Gas Chromatography

OBJECTIVE： To establish a method for the determination of residual N, N-diisopropylethylamine raw material in levocetirizine hydrochloride. METHODS： Headspace gas chromatography was adopted. The determination was performed by headspace gas chromatography on DB-624 column. The heating temperature of vial was 90 ℃, and heating time of it was 15 min. FID detector was adopted using nitrogen as carrier, by temperature programming, and the temperature of detector was 250 %. RESULTS： The linear range of N, N-diisopropylethylamine was 2.01-15.08 μg/ml （r=0.999 3） with average recovery of 98.81% （RSD=l.34%, n：3）. The limits of quantification and detection were 0.201 and 0.101μg/ml. The contents of residual N, N-diisopropylethylamine in 3 batches of samples were 0.006 9%, 0.008 8% and 0.006 3%, respectively. CONCLUSIONS： The method is rapid, sensitive and accurate. It can be used for the content determination of residual N, N-diisopropylethylamine in levocetirizine bydrochloride raw material.