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目的建立测定α-酮亮氨酸钙原料药含量和有关物质的反相离子对色谱方法。方法采用Diamond ODS-C18色谱柱(250 mm×4.6 mm,5μm),流动相:乙腈-0.05 mo.lL-1磷酸二氢钾缓冲液(pH2.5)(体积比为23∶67),内含质量分数为0.1%的氢氧化四丁基铵,流速:1.0 mL.min-1,紫外检测波长:220 nm,柱温:30℃。结果α-酮亮氨酸钙在40~160 mg.L-1内线性关系良好(r=0.999 7),平均回收率为100.4%(RSD=0.71%)。α-酮亮氨酸钙和其有关物质得到良好分离,检测限为16 ng。结论本方法可用于α-酮亮氨酸钙含量测定和有关物质检查。
Objective To establish a reversed-phase ion pair chromatography method for the determination of the content of α-keto leucine and its related substances. Methods The method was performed on a Diamond ODS-C18 column (250 mm × 4.6 mm, 5 μm) with a mobile phase of acetonitrile-0.05 mol·L -1 potassium dihydrogen phosphate buffer (pH 2.5) (volume ratio of 23:67) The mass fraction of 0.1% tetrabutylammonium hydroxide, flow rate: 1.0 mL.min-1, UV detection wavelength: 220 nm, column temperature: 30 ℃. Results The α-keto-leucine calcium showed good linearity (r = 0.999 7) within 40-160 mg · L-1 and the average recovery was 100.4% (RSD = 0.71%). Alpha-keto leucine calcium and its related substances were well separated with a detection limit of 16 ng. Conclusion This method can be used for α-keto leucine calcium content determination and related substances.