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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 a HPLC method for the determination of related substances in raloxifene hydrochloride and its tablets and quantitatively study its main impurities A, C and D. Methods: Venusil XBP C8 column (250 mm × 4.6 mm, 5 μm) was used as the mobile phase A with 0.066 mol·L-1 potassium dihydrogen phosphate buffer (adjusted to pH 3.0 by phosphoric acid). Acetonitrile was used as mobile phase B, Gradient elution, flow rate 1.0 m L · min-1, detection wavelength 280 nm, the qualitative and quantitative analysis of the relevant substances. Results: The raloxifene hydrochloride was separated from each impurity under the selected chromatographic conditions. The detection limits of impurity A, C and D were 21.3, 23.3 and 23.0 ng, respectively, and the concentrations were 0.532 ~ 213.0 and 0.582 ~ 233.0, respectively And 0.538 ~ 215.0μg · m L-1 range and the peak area showed a good linear relationship. Conclusion: The method is simple, sensitive, specific, and has a wide linear range. It can be used for the related substances detection and quality control of raloxifene hydrochloride and its tablets.