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目的:建立罗氟司特(Roflumilast,C17H14Cl2F2N2O3)有关物质和溶剂残留的测定方法。方法:采用高效液相法,以磷酸盐缓冲液(称取磷酸二氢钾0.65 g,加水900 ml,加40%四丁基氢氧化铵水溶液0.5 ml,用磷酸调p H为3.2)-甲醇(90:10)为流动相,对本品进行有关物质测定;采用气相色谱法,DB-624毛细管色谱柱(30 m×0.32 mm×1.80 m),以高纯氮气为载气,检测器为氢火焰离子化检测器(FID),进样口温度为220℃,检测器温度为250℃,以程序升温方式使乙醇达到完全分离。结果:罗氟司特有关物质测定的色谱峰纯度,理论板数,与相邻杂质峰的分离度均达到要求;系统适用性试验、重复性,中间精密度、耐用性均良好;气相测定溶剂残留中,乙醇在该条件下系统适用性,浓度与峰面积线性关系,重复性,回收率,耐用性等良好。结论:采用高效液相法、气相法进行测定,该法操作简便,准确可靠,适用于罗氟司特的质量标准研究。
Objective: To establish a method for the determination of Roflumilast (C17H14Cl2F2N2O3) related substances and solvent residues. Methods: High performance liquid chromatography (HPLC) was carried out using phosphate buffer solution (weighed 0.62 g monobasic potassium phosphate, 900 ml water, 0.5 ml aqueous 40% tetrabutylammonium hydroxide solution and adjusted to pH 3.2 with phosphoric acid) : 10) as the mobile phase, the related substances were determined. The gas chromatography was used on the DB-624 capillary column (30 m × 0.32 mm × 1.80 m) with high purity nitrogen as the carrier gas. The detector was a hydrogen flame Ionization detector (FID), the inlet temperature is 220 ℃, the detector temperature is 250 ℃, temperature is programmed to achieve complete ethanol separation. Results: The chromatographic peak purity, the number of theoretical plates and the separation of the adjacent impurity peaks of the related substances of roflumilast met the requirements. The system suitability test, repeatability, intermediate precision and durability were all good. The gas phase determination solvent Residues, ethanol under the conditions of the system suitability, the linear relationship between concentration and peak area, repeatability, recovery, durability and good. Conclusion: The method is simple, accurate and reliable, and is suitable for the study of the quality standard of roflumilast by HPLC and gas phase method.