RP-HPLC法测定枸橼酸托法替尼含量及有关物质  

Determination of tofacitinib citrate and its related substances by RP-HPLC

作　　者：孙丽娇 吕明明 高爽[1] 孙晓阳[1] 陈明明[2] 陈晓辉[1] 

机构地区：[1]沈阳药科大学药学院,辽宁沈阳110016 [2]沈阳军区药品仪器检验所,辽宁沈阳110026

出　　处：《沈阳药科大学学报》2018年第2期131-137,共7页Journal of Shenyang Pharmaceutical University

摘　　要：目的建立测定枸橼酸托法替尼含量及有关物质的RP-HPLC法。方法使用C18色谱柱(250 mm×4.6 mm,5μm),以乙腈-磷酸盐缓冲液(p H 7.0)为流动相(含量测定采用等度洗脱,体积比25∶75;有关物质测定采用梯度洗脱),流速1.0 m L·min^(-1),检测波长289 nm,柱温30℃。结果在含量测定色谱条件下,托法替尼在质量浓度10.0~60.0 mg·L^(-1)内呈良好线性关系(r=0.999 9),平均回收率为100.5%(n=9);在有关物质测定色谱条件下,托法替尼与各杂质能够得到良好的分离;杂质A^E在质量浓度0.16~1.6 mg·L^(-1),杂质F在质量浓度0.32~1.6 mg·L^(-1)内呈良好的线性关系,杂质A^F的r≥0.999 7。结论该方法可用于枸橼酸托法替尼的含量测定及有关物质的控制。Objective To establish a RP-HPLC method for the determination of tofacitinib citrate and its related substances. Methods The method was performed on a C18 colunm（250 mm ×4. 6 ram,5 μm） using a mobile phase consisting of acetonitrile-phosphate buffer（ pH 7.0） （The content determination used isocratic elution, V： V = 25： 75 ; the impurities determination used gradient elution）. The flow rate was 1.0 mL. min - 1. The detection wavelength was 289 nm and column temperature was 30 ℃. Results For the content determination,the standard curve of tofacitinib was liner in the range of 10. 0 -60. 0 mg·L^-1 （ r =0. 999 9）. The average recovery was 100. 5% （n = 9）. For the impurities determination ,the impurities were completely separated from tofacitinib. The standard curves of impurities A-E were linear in the range of 0. 16 - 1.6 mg·L^-1（r〉0. 999 7）and F was linear in the range of 0. 32 - 1.6 mg·L^-1（r =0. 999 8）. Conclusions The method is suitable for the quality control of tofacitinib and its related substances.

关 键 词：反相高效液相色谱法 托法替尼 有关物质 含量测定 梯度洗脱 

分 类 号：R917[医药卫生—药物分析学]