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SHI Xiaodong,FAN Tian,YAO Jun.Determination of palbociclib by high performance liquid chromatography[J].Journal of Hebei University of Science and Technology,2017,38(4):375-382
高效液相色谱法测定帕布昔利布含量
Determination of palbociclib by high performance liquid chromatography
Received:May 03, 2017  Revised:May 29, 2017
DOI:10.7535/hbkd.2017yx04009
中文关键词:  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
英文关键词:chromatography  palbociclib  HPLC  assay  methodology validation
基金项目:石家庄市科学技术研究与发展计划项目(161200223A)
Author NameAffiliationE-mail
SHI Xiaodong School of Chemical and Pharmaceutical Engineering Hebei University of Science and Technology Shijiazhuang  
FAN Tian School of Chemical and Pharmaceutical Engineering Hebei University of Science and Technology Shijiazhuang  
YAO Jun School of Chemical and Pharmaceutical Engineering Hebei University of Science and Technology ShijiazhuangState Key Laboratory Breeding Base-Key Laboratory of Molecular Chemistry for Drug of Hebei Province Shijiazhuang twobright@163.com 
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中文摘要:
      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。
英文摘要:
      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.
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