学术论文

      高效液相色谱法测定帕布昔利布含量

      Determination of palbociclib by high performance liquid chromatography

      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 C18(250 mm × 4.6 mm,5 μm),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10 μL,检测波长为234 nm,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50~150 μg/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.
      Abstract:
      In order to establish an HPLC method for the content determination of palbociclib, HPLC is performed on the column of Agilent C18 (250 mm × 4.6 mm,5 μm)with the mobile phase of acetonitrile-water (300∶700,0.1% TFA included) at the flow rate of 1.0 mL/min, with the sample size of 10 μL, the detection wavelength of 234 nm and the column temperature of 40 ℃.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 50~150 μg/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 other external factors.It provides a new reference to the content determination of active pharmaceutical ingredients.
      作者: 史校东 [1] 范甜 [1] 姚军 [2]
      Author: SHI Xiaodong [1] FAN Tian [1] YAO Jun [2]
      作者单位: 河北科技大学化学与制药工程学院,河北石家庄,050018 河北科技大学化学与制药工程学院,河北石家庄 050018;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
      刊 名: 河北科技大学学报 ISTICPKU
      年,卷(期): 2017, 38(4)
      分类号: TQ460.7 R917
      在线出版日期: 2017年8月14日
      基金项目: 石家庄市科学技术研究与发展计划项目