HPLC测定盐酸西那卡塞有关物质

Determination of the Related Substances of Cinacalcet Hydrochloride by HPLC

关键词:  盐酸西那卡塞  高效液相色谱法  有关物质

Key words:  cinacalcet hydrochloride  HPLC  related substances

摘要:

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，5 μm),以乙腈-10 mmol·L^-1磷酸二氢钾(用2 mol·L^-1氢氧化钾调pH值至6.5)为流动相进行梯度洗脱，流速为1.0 mL·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~ 4.572 μg·mL^-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 6~4.791 μg·mL^-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 1~5.481 μg·mL^-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 9~2.059 μg·mL^-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。

Abstract:

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 Imp1(r=1.000); the calibration curves were linear in the range of 0.239 6-4.791 μg·mL^-1 for Imp2(r=1.000); the calibration curves were linear in the range of 0.274 1-5.481 μg·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 Imp1, 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.