摘要:
目的 建立了顶空毛细管气相色谱法测定盐酸洛哌丁胺中残留溶剂的方法。 方法 以氮气为载气,氢火焰离子化检测器(FID)检测,色谱柱为DB-624毛细管柱(30 m×0.32 mm×0.25 μm),采用程序升温,顶空进样,顶空平衡温度为100℃,平衡时间25 min。对盐酸洛哌丁胺中甲醇、异丙醇、正己烷、乙酸乙酯、四氢呋喃、氯仿、甲基异丁酮、甲苯、苯这9种有机溶剂残留进行检测。 结果 在试验条件下实现了各组分的分离。甲醇、异丙醇、正己烷、乙酸乙酯、四氢呋喃、氯仿、甲基异丁酮、甲苯、苯在所考察的浓度范围内,线性关系、精密度均良好。各组分平均回收率95.2%~102.3%,RSD 0.8%~2.9%。 结论 该方法简便、准确,可用于盐酸洛哌丁胺中残留溶剂的测定。
Abstract:
Objective To develop a method of headspace capillary gas chromatography for determining residual organic solvents in loperamide hydrochloride. Methods The carrier gas was nitrogen and FID as detector. The nine organic solvents including methanol, isopropanol, n-hexane, ethyl acetate, tetrahydrofuran, chloroform, methyl isobutyl ketone, toluene, benzene were separated on a DB-624 capillary column(30 m×0.32 mm×0.25 μm)by programmable increased temperature and headspace gas chromatography. Results The nine organic solvents were separated and each of them showed linear relationship in the concentration range measured. The recoveries and RSDs were in range from 95.2% to 102.3% and 0.8% to 2.9%, respectively. Conclusion The method was simple, accurate and reproducible.
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