毛细管柱气相色谱法测定盐酸特比萘芬中残留溶剂

Determination of Residual Solvents in Terbinafine Hydrochloride by Gas Chromatography with Capillary Column

摘要: 应用HP-5毛细管柱(25 m×0.32 mm,0.25 μm)气相色谱法测定了盐酸特比萘芬药物中乙醚、异丙醇、乙酸乙酯、三氯甲烷、四氢呋喃、甲苯、二甲基甲酰胺等6种残留溶剂.经烘干的试样溶于二甲替甲酰胺(DMF)中,试样溶液中的残留溶剂经毛细管柱分离后,以苯为内标物,内标法定量测定.6种残留溶剂具有良好的分离效果,整体回收率在92.7%~101.0%之间,相对标准偏差(n=6)在1.5%~2.8%之间,6种残留溶剂检出限(S/N=3)依次为1.5,2.8,2.5,12.0,1.7,1.6 mg·L-1.

Abstract: Gas chromatography with HP-5 capillary column (25 m×0.32 mm,0.25 μm) was applied to the determination of 6 residual solvents,i.e.ethyl ether,iso-propanol,ethyl acetate,chloroform,tetrahydrofuran and toluene,in the propylene drug,terbinafine hydrochloride.The dried sample was dissolved in dimethyformamide (DMF) and the residual solvents in the DMF solution were separated on the capillary column,and determined with FID detector using benzene as internal standard.Values of recovery of the six solvents,as a whole,were in the range from 92.7% to 101.0%.Values of RSD′s (n=6) found were in the range of 1.5%-2.8%.Detection limits (S/N=3) of 1.5,2.8,2.5,12.0,1.7 and 1.6 mg·L-1 were found for the 6 solvents respectively.