药学学报, 2019, 54(4): 710-713
引用本文:
王娜, 戴苏云, 谢梦雨, 马雨璇, 王冰, 李钢. 药物帕博西尼的定性和定量分析研究[J]. 药学学报, 2019, 54(4): 710-713.
WANG Na, DAI Su-yun, XIE Meng-yu, MA Yu-xuan, WANG Bing, LI Gang. Qualitative and quantitative analysis of palbociclib[J]. Acta Pharmaceutica Sinica, 2019, 54(4): 710-713.

药物帕博西尼的定性和定量分析研究
王娜, 戴苏云, 谢梦雨, 马雨璇, 王冰, 李钢
南京师范大学生命科学学院, 分析测试中心, 江苏 南京 210023
摘要:
采用差示扫描量热分析法(differential scanning calorimetry,DSC)、扫描电子显微镜法(scanning electron microscopy,SEM)和X-射线粉末衍射法(X-ray powder diffraction,PXRD)对帕博西尼进行了结构表征,初步建立了帕博西尼A、B两种晶型的鉴定方法;通过X-射线粉末衍射单峰法(峰面积法和峰高法)对帕博西尼(palbociclib)有效晶型A中混杂的晶型B进行了定量测定。结果表明:DSC法鉴定两种晶型其结果区分不够明显,SEM法和PXRD法可快速有效鉴别两种晶型;峰面积法和峰高法所建立的标准曲线方程分别为y=0.842 75x-0.001 21和y=0.909 64x-0.002 32,两种方法的R2值分别为0.986 17和0.985 83,两组曲线均取得了较好的线性关系,其中峰面积法的线性关系更好。峰面积标准曲线计算出B晶型的检测限(limit of detection,LOD)和定量限(limit of quantity,LOQ)分别为1.17%和3.92%,峰高标准曲线计算出B晶型的检测限和定量限分别为1.19%和3.97%,峰面积法更为灵敏。采用本实验的方法可快速的鉴定帕博西尼晶型A和晶型B并对其进行定量测定。
关键词:    帕博西尼      定性分析      定量分析      X-射线粉末衍射     
Qualitative and quantitative analysis of palbociclib
WANG Na, DAI Su-yun, XIE Meng-yu, MA Yu-xuan, WANG Bing, LI Gang
Test and Analysis Center, School of Life Sciences, Nanjing Normal University, Nanjing 210023, China
Abstract:
In this paper, three methods, differential scanning calorimetry (DSC), scanning electron microscopy (SEM) and X-ray powder diffraction (PXRD), were used to characterize the structure of Palbociclib. The form-B crystal mixed in with form-A crystal, the effective form of Palbociclib, was quantitated by the single peak method (peak area method and peak height method) using X-ray powder diffraction. While the qualitative identification by DSC was not clear, SEM and PXRD quickly and effectively identified two types of crystal. The standard curve equations established by the peak area method and the peak height method are:y=0.842 75x-0.001 21 and y=0.909 64x-0.002 32. This suggests that the linear relationship of peak area method is better than that of peak height method (R2=0.986 17 and R2=0.985 83). The sensitivity of the peak area method (LOD=1.17%, LOQ=3.92%) are higher than the peak height method (LOD=1.19%, LOQ=3.97%). The methods from this study can be used to identify and quantify palbociclib form-A and form-B crystal rapidly.
Key words:    palbociclib    qualitative analysis    quantitative analysis    X-ray powder diffraction   
收稿日期: 2018-11-26
DOI: 10.16438/j.0513-4870.2018-1067
基金项目: 江苏省大型科学仪器设备共享服务平台资助(BZ201403).
通讯作者: 王冰, 李钢
Email: 40010@njnu.edu.cn;40388@njnu.edu.cn
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