HPLC法测定盐酸雷洛昔芬及其片剂中的有关物质

HPLC determination of impurities in raloxifene hydrochloride and its tablets

目的：建立盐酸雷洛昔芬及其片剂中有关物质测定的HPLC法,对其主要杂质A、C和D进行定量研究。方法：采用Venusil XBP C8色谱柱（250 mm×4.6 mm,5μm）,以0.066 mol·L^-1磷酸二氢钾缓冲液（磷酸调节p H至3.0）为流动相A,乙腈为流动相B,梯度洗脱,流速1.0 m L·min-1,检测波长280 nm,对有关物质进行定性、定量分析。结果：在选定的色谱条件下,盐酸雷洛昔芬与各杂质分离良好,杂质A、C和D的检测限分别为21.3、23.3和23.0 ng,质量浓度分别在0.532-213.0、0.582-233.0和0.538-215.0μg·m L^-1范围内与峰面积呈良好的线性关系。结论：本方法简便、灵敏,专属性好,线性范围宽,可用于盐酸雷洛昔芬及其片剂的有关物质检测和质量控制。

Objective：To establish an HPLC method for the determination of impurities in raloxifene hydrochloride and its tablets. Methods： The separation was performed on a Venusil XBP C8 column （250 mm × 4. 6 mm, 5 μm） with a mobile phase consisting of a mixture of acetonitrile （mobile phase B） and 0. 066 mol · L^-1 potassium dihydro- gen phosphate buffer （ mobile phase A, pH 3.0） by gradient elution at a flow rate of 1.0 mL ·min ^- 1 The detective wavelength was 280 nm. Results： Raloxifen hydrochloride and its impurities were well separated under the selected liquid chromatographic system. The detection limits of impurity A, C and D were 21.3 ng,23.3 ng,23.0 ng and the calibration curves revealed good linearities over the ranges of 0. 532 -213.0 μg · mL^-1, 0. 582 -233.0 μg ·mL^- 1 and 0. 538 -215.0 μg ·mL^-1. respectively. Conclusion： The method is easy, sensitive, and specific which can be used for the test of the related substances of raloxifene hydrochloride and its tablets and quality control.