摘要
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 an ion-pair RP-HPLC method for the determination of the contents of α-ketoleucine calcium and its related substances.Methods The determination of α-ketoleucine calcium and the separation of its related substances were performed on a C18 column（250 mm×4.6 mm,5 μm）.The mobile phase was acetonitrile-0.05%（w）potassium dihydrogen phosphae（pH2.5）（V∶V=23∶67）with 0.01%（w）tetrabutyl ammonium hydroxide.The flow rate was 1.0 mL·min-1.Ultraviolet absorption detector was set at 220 nm with column temperature at 30 ℃.Results The linear range of α-ketoleucine calcium was between 40 and 160 mg·L-1（r=0.999 7）.The average recovery was 100.4%（w）with RSD of 0.7%.The related substances of α-ketoleucine calcium could be completely separated from α-ketoleucine calcium.The limit of detection（LOD）was 16 ng.Conclusion The method is simple and accurate for quality control of the α-ketoleucine calcium.
出处
《沈阳药科大学学报》
CAS
CSCD
北大核心
2011年第4期291-294,315,共5页
Journal of Shenyang Pharmaceutical University
