高效液相色谱法测定帕布昔利布含量  

Determination of palbociclib by high performance liquid chromatography

作　　者：史校东 范甜[1] 姚军[1,2] 

机构地区：[1]河北科技大学化学与制药工程学院,河北石家庄050018 [2]河北省药用分子化学重点实验室-省部共建国家重点实验室培育基地,河北石家庄050018

出　　处：《河北科技大学学报》2017年第4期375-382,共8页Journal of Hebei University of Science and Technology

基　　金：石家庄市科学技术研究与发展计划项目(161200223A)

摘　　要：为建立帕布昔利布(PD)含量测定方法,采用高效液相色谱法,色谱柱为Agilent HC C_(18)(250mm×4.6mm,5μm),流动相为乙腈-水(二者体积比为300∶700,含0.1%(体积分数)三氟乙酸),流速为1.0 mL/min,按照等度洗脱,进样量为10μL,检测波长为234nm,柱温为40℃。结果表明:主药与各杂质之间分离度良好;帕布昔利布质量浓度在50~150μg/mL范围内与峰面积线性关系良好,r为0.999 5;仪器精密度、中间精密度、稳定性试验的RSD值小于2.0%;帕布昔利布回收率为100.0%,RSD值为0.8%(n=9)。本方法可以准确快速测定PD含量,有效排除其他外界因素的影响,为帕布昔利布原料药含量测定提供新的参考。In order to establish an HPLC method for the content determination of palbociclib,HPLC is performed on the column of Agilent C（18）（250mm × 4.6mm,5μm）with the mobile phase of acetonitrile-water（300∶700,0.1% TFA included）at the flow rate of 1.0mL/min,with the sample size of 10μL,the detection wavelength of 234 nm and the column temperature of40 ℃.The result shows that the main drug and the related substances could be well separated;the calibration curve of palbociclib is in good linearity over the range of 50-150μg/mL,and r=0.999 5;the RSD of instrument precision,intermediate precision and stability test of related substances and content are no more than 2.0%;the average recovery is 100.0% with RSD of 0.8%（n=9）.The method can rapidly and accurately determine the PD content,effectively eliminate the effects of otherexternal factors.It provides a new reference to the content determination of active pharmaceutical ingredients.

关 键 词：色谱分析 帕布昔利布 高效液相色谱法 含量测定 方法学验证 

分 类 号：TQ460.7[化学工程—制药化工] R917[医药卫生—药物分析学]