顶空气相色谱法同时测定盐酸左西替利嗪原料药中的3种残留溶剂

Simultaneous determination of 3 residual organic solvents in the raw material of levocetirizine hydrochloride by HS-GC

目的建立同时测定盐酸左西替利嗪原料药中甲醇、三乙胺、N,N-二异丙基乙胺3种有机溶剂残留量的方法。方法采用顶空气相色谱法(HS-GC),Restek Rxi-624sil MS(30 m×0.32 mm×1.8μm)色谱柱,程序升温,分流进样,氢火焰离子化检测器,流速:2.0 mL·min-1,顶空瓶加热温度90℃,保持15 min,外标法定量。结果在本色谱条件下,3种残留溶剂均能得到良好的分离,空白溶剂无干扰,且在一定的浓度范围内均具有良好的线性关系,r在0.9995～1.000;平均加样回收率均在91.2%～108.6%(RSD均小于3.0%,n=3)。结论该方法灵敏度、准确度均达到有机溶剂残留量的检测要求,专属性强、重复性好、回收率高,可用于盐酸左西替利嗪原料药中残留溶剂的分析检测。

Objective To establish a method for the simultaneous determination of 3residual organic solvents of methanol,triethylamine and N,N-diisopropylethylamine in levoeetirizine hydrochloride.Methods Headspace gas chromatography (GS-GC)was adopted.The determination was performed on a column Restek Rxi'-624sil MS (30m×0.32mm × 1.8μm)with programmed temperature.Split injection and inlet temperature was 200℃. Hydrogen flame ionization detector was used with 250℃.Nitrogen was used as the carder gas at 2.0mL·min^-l. The headspace equilibrium temperature was 90℃,and equilibrium time was 5min.External standard was used for the content determination.Results Under this chromatographic condition,the 3kinds of residual solvents were well separated,the blank solvent showed no interference,and residual solvents had good linear relationship in a certain concentration range,r was 0.9995--1.000.The average recoveries were at 91.2%--108.6%and the relative standard deviations of recoveries (n =3)were lower than 3.0%.Conclusion The sensitivity and accuracy of this method all meet the detection requirements of organic solvent residues,and the method is highly specificy,and repeatable with high recovery.It can be used for the analysis and determination of residual solvents in levocetirizine hydrochloride.