顶空气相色谱法测定丁苯酞原料药中6种有机溶剂残留量

Determination of six residual solvents in butylphthalide by headspace gas chromatography

采用顶空气相色谱法对丁苯酞原料药中的甲醇、乙腈、二氯甲烷、乙酸乙酯、四氢呋喃和正庚烷共6种残留溶剂的含量进行测定.使用Agilent DB-624(0.32 mm×30 m,3μm)色谱柱,色谱柱程序升温;氢火焰离子化检测器,检测器温度为250℃.进样口温度为220℃;顶空平衡温度为80℃,平衡时间为30 min.结果显示,6种残留溶剂间分离度良好.在一定质量浓度范围内,各残留溶剂线性关系均良好,相关系数r>0.9990.重复性实验结果的相对标准偏差值均小于5%,加样回收率均在80%~120%范围内,不同批次原料药残留溶剂检查结果均符合要求.该方法准确灵敏,可用于丁苯酞原料药中残留溶剂的测定.

A headspace gas chromatography(GC)method was developed for the analysis of six residual solvents in butylphthalide,the residual solvents including methanol,acetonitrile,dichloromethane,ethyl acetate,tetrahydrofuran and n-heptane.Separation was performed on a DB-624 capillary column(0.32 mm×30 m,3μm)using a column temperature programming.Flame ionization detector was used as the detector.The detector temperature and the inlet temperature were 250℃ and 220℃ respectively.The headspace temperature was 80℃ and the equilibrium time was 30 min.6 residual solvents were separated very well.The linearity of the 6 residual solvents were perfect ranged from 10%-150% of their limit concentration(r>0.9990).The relative standard deviations of repeatability results were all less than 5%.The average recoveries were in the range of 80%-120%.The residual solvents results of different batches of butylphthalide were in accordance with the requirements.This method is accurate and sensitive,and it can be used for the determination of the residual solvents in butylphthalide.