毛细管气相色谱法测定13种有机溶剂残留

Determination of thirteen residue organic solvents by capillary gas chromatography in two injector types

目的建立药物中残留溶剂正戊烷、正己烷、甲醇、乙醇、乙腈、丙酮、乙酸乙酯、二氯甲烷、四氢呋喃、吡啶、甲苯、N,N-二甲基甲酰胺和乙酸的毛细管气相色谱测定方法,并比较顶空进样与溶液直接进样两种进样方式的差异。方法采用毛细管气相色谱法,以两种不同的进样方式,色谱柱为HP-InnoWax毛细管柱(键合聚乙二醇PEG,30m×320μm×0.50μm)及DM-624(6%氰基甲基硅酮)毛细管柱(30m×530μm×3.00μm),载气为氮气,检测器为氢焰离子化检测器,以程序升温顶空进样方式使甲醇、乙醇、乙腈、丙酮、乙酸乙酯、二氯甲烷、四氢呋喃、吡啶和甲苯在HP-InnoWax毛细管柱上实现了完全分离;以溶液直接进样方式使正戊烷、正己烷、DMF和乙酸在DM-624毛细管柱上达到了完全分离。结果两种进样方式中各溶剂的线性关系、精密度、准确度、灵敏度均达到了《中国药典》2010版中残留溶剂限量规定的测定要求。结论建立的方法能快速准确地检测13种有机溶剂,并可用于药物质量控制中的有机残留溶剂检查。

Objective To establish a capillary gas chromatography（GC） method for determination of thirteen residual organic solvents in drugs and to compare the difference between two injector types.Methods A capillary GC method was established with FID detector.The capillary columns were HP-InnoWax（30 m×320 μm×0.50 μm） and DM-624（30 m×530 μm×3.00 μm）.The injection modes were headspace injector and direct injector.Nitrogen was used as carrier gas.Nine of 13 organic solvents including acetone,4H-furan,acetic ether,methanol,dichlormethane,ethanol,acetonitrile,methylbenzene,and pyridine were completely separated by using gradient temperature program on HP-InnoWax with headspace injector.While n-pentane,n-hexane,DMF and acetic acid were also well separated by using temperature program on DM-624 with GC injector.Results The linearity,precision,accuracy and sensitivity of the thirteen solvents under condition of this method were complied with the analytical requirements of residual organic solvents in Chinese pharmacopoeia.Conclusions This method（GC） is rapid and accurate to determine the thirteen solvents as the residue organic solvent in drugs.