目的 建立了測定非布司他原料藥中可能殘留的7種有機(jī)溶劑（甲醇、乙醇、異丙醇、二氯甲烷、四氫呋喃、正庚烷、氯苯）的檢測方法。方法 采用頂空氣相色譜法，色譜柱為DB-624毛細(xì)管柱（30.0 m×0.53 mm×3.00 μm），載氣為高純氮?dú)?；頂空溫度?0 ℃，頂空時間為30 min；柱溫50 ℃，維持2 min，以10 ℃/min升至200 ℃，維持2 min；氫火焰離子化檢測器（FID），溫度為250 ℃。結(jié)果 在考察的濃度范圍內(nèi)線性關(guān)系良好（r=0.998 0～0.999 8），7種殘留溶劑均完全分離，精密度、重復(fù)性試驗(yàn)RSD值均小于5.0%，被測組分的平均回收率符合規(guī)定，供試品溶液穩(wěn)定。結(jié)論 該氣相色譜法操作簡便，準(zhǔn)確，靈敏度高，可用于檢測非布司他原料藥中有機(jī)溶劑的殘留物。

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 × 0.53 mm × 3.00 μm). The initial temperature was kept at 50 ℃ for 2 min, then the temperature was raised to 200 ℃ at the rate of 10 ℃/min and subsequently sustained for 2 min. FID detector temperature was 250 ℃. The vial temperature was 80 ℃, 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.