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目的建立依普利酮含量和有关物质的反相高效液相色谱测定方法。方法色谱柱为Agilent Poroshell色谱柱(4.6mm×100 mm,2.7μm),流动相为0.1%磷酸溶液-乙腈-甲醇(64∶18∶18),流速为1.0 m L·min-1,检测波长为240 nm;稀释剂为水-乙腈-甲醇(50∶25∶25)。结果有关物质:依普利酮峰与其他杂质峰可以良好分离;依普利酮、中间体Ⅲ和Ⅳ、有关物质A~E的检测限分别为0.03、0.13、0.25、0.05、0.05、0.26、0.07和0.12 ng,定量限分别为0.12、0.42、0.84、0.18、0.18、0.86、0.22和0.41 ng;依普利酮和有关物质A~E分别在0.13~1.53、0.25~3.03、0.25~2.99、0.13~1.61、0.14~1.63和0.13~1.54μg·m L-1内线性关系良好(r=0.999 9,n=7),且有关物质A~E相对依普利酮的校正因子均在0.90~1.10之间;有关物质A~E的平均加样回收率(n=9)均在95.0%~105.0%之间。含量测定:依普利酮在12.60~75.63μg·m L-1内线性关系良好(r=0.999 6,n=6),且重复性好(RSD=0.19%,n=6)。结论本法简便、灵敏度高、专属性强、准确度和精密度好,可以用于依普利酮含量和有关物质测定。
Objective To establish a method for the determination of eplerenone and related substances by reversed-phase high performance liquid chromatography. Methods The column was Agilent Poroshell column (4.6 mm × 100 mm, 2.7 μm) with a mobile phase of 0.1% phosphoric acid solution-acetonitrile-methanol (64:18:18) at a flow rate of 1.0 m L · min- Was 240 nm; the diluent was water-acetonitrile-methanol (50:25:25). Results Related substances: Eplerenone peak was well separated from other impurity peaks; the detection limits of related substances A ~ E were less than 0.03,0.13,0.25,0.05,0.05,0.26, 0.07 and 0.12 ng respectively. The limits of quantitation were 0.12, 0.42, 0.84, 0.18, 0.18, 0.86, 0.22 and 0.41 ng respectively. Eplerenone and related substances A ~ E were 0.13 ~ 1.53,0.25 ~ 3.03,0.25 ~ 2.99, 0.13 ~ 1.61, 0.14 ~ 1.63 and 0.13 ~ 1.54μg · m L-1 (r = 0.999 9, n = 7), and the correction factors of relative substance E to eplerenone were all within the range of 0.90 ~ 1.10; The average recoveries of related substances A ~ E (n = 9) ranged from 95.0% to 105.0%. Determination of content: Eplerenone in 12.60 ~ 75.63μg · m L-1 good linear relationship (r = 0.999 6, n = 6), and good repeatability (RSD = 0.19%, n = 6). Conclusion This method is simple, high sensitivity, specificity, accuracy and precision, and can be used for determination of eplerenone content and related substances.