顶空气相色谱法测定非布司他原料药中有机溶剂残留

目的建立了测定非布司他原料药中可能残留的7种有机溶剂（甲醇、乙醇、异丙醇、二氯甲烷、四氢呋喃、止庚烷、氯苯）的检测方法。方法采用顶空气相色谱法，色谱柱为DB-624毛细管柱（30．0m×0．531Tim×3．00μm），载气为高纯氮气；顶空温度为80℃，顶空时间为30min；柱温50℃，维持2min，以10℃／min升至200℃，维持2min；氢火焰离子化检测器（FID），温度为250℃。结果在考察的浓度范围内线性关系良好（r=0．9980-0．9998），7种残留溶剂均完全分离，精密度、重复性试验RSD值均小于5．0％，被测组分的平均回收率符合规定，供试品溶液稳定。结论该气相色谱法操作简便，准确，灵敏度高，可用于检测非布司他原料药中有机溶剂的残留物。

Determination of residual organic solvents in febuxostat bulks drug by headspace gas chromatography

Objective To establish a method for determination of the seven residual organic solvents, such as methanol, ethanol, isopropanol, dichloromethane, tetrahydrofuran, n-heptane, and chlorobenzene in febuxostat bulks drug. Methods Gas headspace chromatography was applied to the study. The column was DB-624 silica capillary column （30：0 m x 0.53 mm x 3.00 μm）. The initial temperature was kept at 50 °C for 2 min, then the temperature was raised to 200 °C at the rate of 10 °C/min and subsequently sustained for 2 min. FID detector temperature was 250 °C. The vial temperature was 80 °C, and the vial time was 30 min. Results There was a good linearity in the experimental concentration （r =0.998 0 - 0.999 8）. The RSD values were all less than 5.0%. The average recovery was good. The test solution was stable. Conclusion The analytical method is simple, accurate and sensitive, which could be used for the quality control of residual organic solvents in febuxostat bulks drug.