HPLC法分析醋酸阿比特龙原料有关物质

HPLC Analysis of Related Substances in Raw Material of Abiraterone Acetate

目的采用HPLC法研究醋酸阿比特龙原料药中的有关物质,为醋酸阿比特龙原料质量控制提供依据。方法用ProntoSIL C18色谱柱(3 mm×150 mm,3μm),流动相A[10 mmol/L乙酸铵-乙腈(95∶5)],流动相B(乙腈),流动相C(乙醇),采用梯度洗脱程序,流速是0.35 mL/min,柱温是15℃,检测波长是254 nm,进样量是10μL;对醋酸阿比特龙中杂质进行分离。结果主峰、各已知杂质与相邻杂质之间分离度均不小于1.5;主峰及各杂质分别在0.0497μg/mL~1.9863μg/mL,0.0506μg/mL~2.0229μg/mL,0.0317μg/mL~2.1166μg/mL,0.3013μg/mL~2.0087μg/mL,0.2988μg/mL~1.9917μg/mL,0.0821μg/mL~2.0529μg/mL,0.0988μg/mL~1.9767μg/mL,0.0773μg/mL~1.9319μg/mL范围内呈良好的线性关系。各杂质回收率均在91.49%~106.00%,9份回收率RSD值均在1.79%~4.35%。经测定3批样品中杂质A,B,C,D,E,G含量均符合规定,杂质F均未检出,总杂含量分别为0.14%、0.11%、0.13%。结论HPLC法准确性高、灵敏度高、重复性好,适用于醋酸阿比特龙中有关物质测定。

Objective To study the related substances in the raw material of abiraterone acetate by HPLC,and provide a basis for the quality control of this product.Methods Using a ProntoSIL C18 chromatographic column(3 mm×150 mm,3μm),mobile phase A[10 mmol/L ammonium acetate acetonitrile(95:5)],mobile phase B(acetonitrile),mobile phase C(ethanol),using a gradient elution program,flow rate of 0.35 mL/min,column temperature of 15℃,detection wavelength of 254 nm,injection volume of 10μL;separation of impurities in abiraterone acetate.Results The separation degree between the main peak,known impurities,and adjacent impurities is not less than 1.5;the main peak and various impurities showed a good linear relationship within the range of 0.0497μg/mL~1.9863μg/mL,0.0506μg/mL~2.0229μg/mL,0.0317μg/mL~2.1166μg/mL,0.3013μg/mL~2.0087μg/mL,0.2988μg/mL~1.9917μg/mL,0.0821μg/mL~2.0529μg/mL,0.0988μg/mL~1.9767μg/mL,0.0773μg/mL~1.9319μg/mL.At three concentration levels of 50%,100%,and 150%,the recovery rates of each impurity are between 91.49%and 106.00%,and the RSD values of the nine recoveries are all between 1.79%and 4.35%.After testing,the content of impurities A,B,C,D,E,and G in three batches of samples met the requirements.Impurity F was not detected,and the total impurity content was 0.14%,0.11%,and 0.13%,respectively.Conclusion The HPLC method has high accuracy,sensitivity,and repeatability,and is suitable for the accurate determination of the content of related substances in abiraterone acetate.