HPLC测定盐酸西那卡塞有关物质

Determination of the Related Substances of Cinacalcet Hydrochloride by HPLC

目的建立高效液相色谱法测定盐酸西那卡塞有关物质。方法采用Waters C18色谱柱（250 mm×4.6 mm,5μm）,以乙腈-10 mmol·L^-1磷酸二氢钾（用2 mol·L^-1氢氧化钾调p H值至6.5）为流动相进行梯度洗脱,流速为1.0 m L·min^-1,检测波长为210 nm。结果各杂质与主峰之间的分离度良好。4个已知杂质：R-1-（1-萘基）乙胺（Imp1）浓度在0.228 6-4.572μg·m L？1内与峰面积呈良好的线性关系,r为1.000;3-（三氟甲基）苯丙醇（Imp2）浓度在0.239 6-4.791μg·m L？1内与峰面积呈良好的线性关系,r为1.000;3-（3-（三氟甲基）苯基）丙基甲磺酸酯（Imp3）浓度在0.274 1-5.481μg·m L^-1内与峰面积呈良好的线性关系,r为1.000;R-N-（1-（萘-1-基）乙基）-3-（3-（三氟甲基）苯基）-N-（3-（三氟甲基）苯基）丙基-1-胺（Imp4）浓度在0.102 9-2.059μg·m L^-1内与峰面积呈良好的线性关系,r为0.999 8;Imp1、Imp2、Imp3和Imp4加样回收率的平均值分别为99.3%,98.9%,99.0%和100.4%;RSD分别为1.8%,2.9%,1.7%和1.7%。结论本方法简便、准确可靠,适用于盐酸西那卡塞中有关物质的控制。

OBJECTIVE To establish an HPLC method for determining the contents of the related substances of cinacalcet hydrochloride. METHODS The condition of detection were： Waters C18 column （250 mm×4.6 mm,5μm）, the gradient mobile phase consisted of acetonitrile and 10 mmol·L^-1 potassium dihydrogen phosphate （adjust with 2 mol·L^-1 potassium hydroxide to pH 6.5） with a flow rate of 1.0 mL·min^-1, the UV detection wavelength was 210 nm. RESULTS The resolution of cinacalcet hydrochloride and relate substances was good. The calibration curves were linear in the range of 0.228 6-4.572 μg·mL^-1 for Impl（r=1.000）; the calibration curves were linear in the range of 0.239 6-4.791 μg.mL-l for Imp2（r=1.000）; the calibration curves were linear in the range of 0.274 1-5.481μg·mL^-1 for Imp3（r=1.000）; the calibration curves were linear in the range of 0.102 9-2.059 μg·mL^-1 for Imp4（r=0.999 8）. The average recoveries of Impl, Imp2, Imp3 and Imp4 were 99.3%, 98.9%, 99.0% and 100.4% respectively; the RSD were 1.8%, 2.9%, 1.7% and 1.7% respectively. CONCLUSION The method is simple, accurate, reliable and can be used for the quality control of the related substances of cinacalcet hydrochloride.