Objective: To develop a method to determine the content of impurity Ⅰ and impurity Ⅱ in lanthanum carbonate raw materials by X-ray powder diffraction, and provide a simple, convenient and feasible quantitative analysis method for the stability research and quality control of lanthanum carbonate drugs. Methods: Single peak method, the detection sensitivity was improved by optimizing the detection parameters, and the characteristic diffraction peak of impurity I was 2θ=17.8 ° and characteristic diffraction peak of impurity Ⅱ was 2θ=26.1 °. The height of diffraction peak was used as the quantitative parameter, and the linear relationship between the peak height and impurity content was established. The content of impurity I and impurity Ⅱ in lanthanum carbonate API samples were determined by the standard curve method. By optimizing the hybrid method, the repeatability of the method was improved. Results: The heights of characteristic diffraction peaks of impurity Ⅰ and impurity Ⅱ showed a good linear relationship with their content. The detection limits of impurity Ⅰ and impurity Ⅱ were 0.55% and 0.29%, respectively. The linear range of impurity Ⅰ was 0.55%-5.06%, the linear equation was Y=408.77X-103.8, and the correlation coefficient r=0.992 1. The linear range of impurity Ⅱ was 0.29%-5.12%, the linear equation square was Y=816.95X-182.52, and the correlation coefficient r=0.996 0. The accuracy of impurity Ⅰ and impurity Ⅱ were 95.9% and 96.1% respectively, and the RSD of repeatability were 6.8% and 7.1% respectively. The contents of impurity Ⅰ and impuriyt Ⅱ in the three batches of samples were lower than the corresponding detection limit. Conclusion: The quantitative method established in this study is accurate, reliable, fast and simple, and can be used for the quantitative analysis of two impurities in lanthanum carbonate raw materials.
JING Yi-wen, AN Yang, ZHANG Ting-ting, GUO Wei, ZHANG Wei-feng, XIAO Chao-qiang, HE Shu-wang
. Quantitative analysis of two impurities in lanthanum carbonate by X-ray powder diffraction[J]. Chinese Journal of Pharmaceutical Analysis, 2023
, 43(4)
: 660
-667
.
DOI: 10.16155/j.0254-1793.2023.04.15
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