摘要
目的:四水碳酸镧(La_(2)(CO_(3))_(3)·4H_(2)O)作为治疗高磷血症的重要药物,在其生产过程中极易引入碱式碳酸镧(LaCO_(3) OH)杂质,为了确保仿制药生产的质量,要对其建立定性和定量分析的方法。方法:采用X射线粉末衍射(PXRD)、热重-差热分析法(TG-DTA)、傅里叶变换红外光谱(FTIR)等现代分析手段进行定性分析并且通过扫描电子显微镜(SEM)观察不同样品的形貌。在PXRD定性分析的基础上,对四水碳酸镧中碱式碳酸镧的两种杂质晶型进行定量分析,通过选取3个物相特征峰计算绘制两种杂质晶型的标准曲线。结果:PXRD、TGA、IR、SEM可快速鉴别四水碳酸镧、碱式碳酸镧I和II 3种晶型物相,定量分析采用峰面积法建立的标准曲线表现出更好的线性关系(碱式碳酸镧晶型I:R^(2)=0.98431;碱式碳酸镧晶型II:R^(2)=0.98933)。结论:上述方法能对四水碳酸镧、碱式碳酸镧I和II3种晶型物相起到快速鉴定和定量测定的作用,具有一定的实践和理论参考意义。
As an important drug in the treatment of hyperphosphatemia,lanthanum carbonate tetrachloride(La_(2)(CO_(3))_(3)·4H_(2)O)is easy to introduce basic lanthanum carbonate(LaCO_(3) OH)in the production process.The samples were qualitatively identified by modern analytical means,such as X-ray powder diffraction(PXRD),thermogravimetric differential thermal analysis(TG-DTA),Fourier transform infrared spectroscopy(FTIR),and the morphology of different samples were observed by scanning electron microscopy(SEM).Based on the qualitative analysis of PXRD,the two crystal forms of basic lanthanum carbonate impurities in lanthanum carbonate tetrachloride were quantitatively analyzed,and the standard curves of the crystal forms of the two impurities were drawn by selecting three phase characteristic peaks.The results showed that PXRD,TGA,IR,SEM could quickly confirm La_(2)(CO_(3))_(3)·4H_(2)O,LaCO_(3) OH-I and LaCO_(3) OH-II,the standard curve established by the peak-area method showed a better linear relationship(LaCO_(3) OH-I:R^(2)=0.98431;LaCO_(3) OH-II:R^(2)=0.98933).This method has practical and theoretical significance.
作者
马雨璇
王娜
李钢
Ma Yuxuan;Wang Na;Li Gang(Test&Analysis Center of School of Food Sciences and Pharmaceutical Engineering,Nanjing Normal University,Nanjing 210023,China)
出处
《分析仪器》
CAS
2021年第4期102-110,共9页
Analytical Instrumentation
关键词
四水碳酸镧
碱式碳酸镧
定性分析
定量分析
X-射线粉末衍射法
La_(2)(CO_(3))_(3)·4H_(2)O
LaCO_(3)OH
Qualitative analysis
Quantitative analysis
X-ray powder diffraction
