氧氟沙星中有机溶剂残留量的气相色谱分析

Determination of residual organic solvents in ofloxacin by GC

通过实验建立氧氟沙星原料药中有机溶剂残留量的毛细管气相色谱分析的测定方法。采用的色谱柱为RTX-5,进样口温度:170℃,检测器温度:250.0℃;柱温:程序升温,初始温度35℃,保持5min,以5℃.min-1升温至60℃,保持5min,再以55℃.min-1升温至230℃,保持5min。载气:N2,分流比:20:1,尾吹流量:30.0mL.min-1。采用内标法和外标法分别分析甲醇、二氯甲烷、乙腈、乙酸乙酯、四氢呋喃、吡啶7种有机物的残留量,以N,N-二甲基甲酰胺为溶剂。此分析方法下待测物均能得到很好的分离,峰面积与浓度成良好的线性关系,精密度良好。可以用于氧氟沙星药品中有机溶剂残留量的测定。

A method for detection of the residual solvents in ofloxacin was established. The residual solvents in Ofloxacin were determined by GC with RTX-5 capillary column, and using nitrogen as carrier gas. The injector temperature was 170 ℃ and the detector temperature was 250 ℃. The column temperature was raised by program, the initial temperature was 35℃, maintained for 5 min, raised to 60 ℃ with a rate of 5 ℃ ·min^-1, maintained for 5 min, then raised to 230℃ with a rate of 55 ℃·min^-1, and maintained for 5 min. The split ratio was 20：h The make-up gas rate was 30 mL·min^-1 Internal standard method and external standard method were adopted to detecting the residual of carbinol, dichloromethane, acetonitri, ethyl acetate, tetrahydrofuran, pyridine. The solvents can be completely separated and the calibration curves of each solvent showed good linear relationship within a certain range. The method is accurate and reliable. It can be applied in detection of residual solvents in ofloxacin.