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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、正庚烷、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(30.0 m×0.53 mm×3.00μm),载气为高纯氮气;顶空温度为80℃,顶空时间为30 min;柱温50℃,维持2 min,以10℃/min升至200℃,维持2 min;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=0.998 0~0.999 8),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。
OBJECTIVE To establish a method for the determination of 7 organic solvents (methanol, ethanol, isopropanol, methylene chloride, tetrahydrofuran, n-heptane and chlorobenzene) that may remain in febuxostat. Methods The headspace gas chromatography was used. The column was DB-624 capillary column (30.0 m × 0.53 mm × 3.00 μm). The carrier gas was high purity nitrogen. The headspace temperature was 80 ℃ and the headspace time was 30 min. 50 ℃, maintained for 2 min, with 10 ℃ / min rose to 200 ℃, for 2 min; hydrogen flame ionization detector (FID), the temperature was 250 ℃. The results showed good linearity (r = 0.998 0 ~ 0.999 8) within the investigated concentration range. The seven residual solvents were completely separated. The RSD values of the precision and reproducibility tests were all less than 5.0%. The average recoveries of the tested components were in agreement Provisions for the test solution stability. Conclusion The gas chromatography is simple, accurate and sensitive. It can be used to detect the residues of organic solvents in febuxostat.