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目的:建立项空气相色谱测定药物硝唑尼特中残留溶剂的方法。方法:采用DM-WAX毛细管色谱柱(30 m×0.25 mm,0.5μm);枉温采取程序升温;进样口温度为200℃;FID检测器,检测器温度为250℃;顶空进样,平衡温度为80℃,平衡时间为30 min;以N,N-二甲基甲酰胺为溶剂测定硝唑尼特原料药中丙酮、二氯甲烷的残留量。结果:在本文的色谱条件下,各有机溶剂均能得到有效分离,丙酮、二氯甲烷的浓度分别在250～750μg·ml~(-1)(r=0.999 1)、30～90μg·ml~(-1)(r=0.999 1)范围内线性关系良好;平均回收率分别为99.15%、99.18%,RSD分别为2.17%、2.97%(n=9)。结论:本方法简便、快速、准确,可有效检测硝唑尼特中的残留溶剂。
OBJECTIVE: To establish a method for the determination of residual solvents in drug nitazoxanide by air chromatography. Methods: DM-WAX capillary column (30 m × 0.25 mm, 0.5 μm) was used. The temperature was programmed to increase in temperature. The temperature of inlet was 200 ℃. The temperature of FID detector was 250 ℃. The equilibrium temperature was 80 ℃, and the equilibration time was 30 min. The residues of nitazoxanide in acetone and dichloromethane were determined by using N, N-dimethylformamide as the solvent. Results: Under the chromatographic conditions, the organic solvents could be separated effectively. The concentrations of acetone and dichloromethane were in the ranges of 250 ~ 750μg · ml -1 (r = 0.999 1), 30 ~ 90μg · ml ~ (-1) (r = 0.999 1). The average recoveries were 99.15% and 99.18%, respectively, with RSDs of 2.17% and 2.97%, respectively (n = 9). Conclusion: The method is simple, rapid and accurate, and can effectively detect residual solvents in nitazoxanide.