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目的采用RP-HPLC和Chiral-HPLC法测定赛洛多辛中的有关物质和对映异构体。方法采用Kromasil C8色谱柱(250 mm×4.6 mm,5μm)检查有关物质,流动相为0.01 mol.L-1磷酸二氢铵溶液(三乙胺调pH6.8)-乙腈(66∶34),检测波长为225 nm。采用Chiralpak AD-H手性柱(250 mm×4.6 mm,5μm)检查赛洛多辛对映异构体,流动相为正己烷-乙醇-二乙胺(55∶45∶0.05),流速为0.5 mL.min-1,检测波长为220 nm。结果主峰与相邻杂质峰能很好地分离,赛洛多辛的检测限、定量限分别为11.1、33.3 ng。异构体检查中,赛洛多辛与其对映体的分离度可达5.0,其对映体在0.15～15.35μg.mL-1具有良好的线性关系(r=0.9999)。结论所用方法简便准确、重复性好,适用于赛洛多辛的质量控制。
OBJECTIVE To determine the related substances and enantiomers of silodosin by RP-HPLC and Chiral-HPLC. Methods Kromasil C8 column (250 mm × 4.6 mm, 5 μm) was used to check the contents of the substance. The mobile phase consisted of 0.01 mol·L-1 ammonium dihydrogen phosphate solution (triethylamine adjusted to pH6.8) -acetonitrile (66:34) The detection wavelength is 225 nm. The enantiomers of silodosin were checked on a Chiralpak AD-H chiral column (250 mm × 4.6 mm, 5 μm) using n-hexane-ethanol-diethylamine (55:45:0.05) at a flow rate of 0.5 mL.min-1, the detection wavelength was 220 nm. Results The main peak and adjacent impurity peaks were well separated. The detection limit and the limit of quantification of silodosin were 11.1 and 33.3 ng, respectively. In the isomer examination, the separation of sildoluxin and its enantiomer was up to 5.0, and its enantiomer had a good linear relationship (r = 0.9999) at 0.15 ~ 15.35μg.mL-1. Conclusion The method is simple, accurate and reproducible, which is suitable for the quality control of silodosin.