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目的:用X-射线粉末衍射法测定埃索美拉唑镁三水合物和二水合物A晶型混合物中晶型的含量,为埃索美拉唑镁晶型药物的质量控制提供一种切实可行的晶型定量分析方法。方法:采用X-射线粉末衍射法表征埃索美拉唑镁盐三水合物晶型和二水合物A晶型。分别选择埃索美拉唑镁三水合物的特征衍射峰2θ=5.27°(I/I0=100%)和二水合物A晶型的特征衍射峰2θ=5.65°(I/I0=100%)的峰面积比值为定量参数,建立标准曲线,测定埃索美拉唑镁原料中三水合物晶型和二水合物A晶型的含量。结果:埃索美拉唑镁二水合物A晶型的特征衍射峰和三水合物的特征衍射峰的峰面积比值与三水合物的含量呈良好的线性关系,在三水合物含量为3%~15%的范围内,得到的标准曲线为Y=0.004 3X+0.313 6;Y为特征衍射峰的峰面积比,X为三水合物的质量分数,相关系数r=0.999 6;方法精密度为2.4%;运用标准曲线对三水合物含量为5.48%、10.33%、12.49%的样品进行定量分析,结果表明测得值与真实值之间的绝对误差分别为0.14%、0.01%、0.06%。结论:所建方法准确可靠,快速简便,可用于埃索美拉唑镁原料中三水合物晶型和二水合物A晶型的定量分析。
OBJECTIVE: To determine the content of crystalline form of esomeprazole magnesium trihydrate and dihydrate A crystal mixture by X-ray powder diffractometry and to provide a practical solution for the quality control of esomeprazole magnesium crystalline drug Feasible crystal form quantitative analysis method. Methods: X-ray powder diffraction method was used to characterize the esomeprazole magnesium salt trihydrate crystal form and dihydrate A crystal form. The characteristic diffraction peaks 2θ = 5.27 ° (I / I0 = 100%) and the characteristic diffraction peak 2θ = 5.65 ° (I / I0 = 100%) of the crystal form of dihydrate A were selected respectively for esomeprazole magnesium trihydrate. Of the peak area ratio as a quantitative parameter to establish a standard curve to determine the esomeprazole magnesium raw material trihydrate form and dihydrate Form A content. Results: The peak area ratio of characteristic diffraction peak of esomeprazole magnesium dihydrate Form A and the characteristic diffraction peak of trihydrate showed a good linear relationship with the content of trihydrate. When the content of trihydrate was 3% ~ 15%, the standard curve obtained is Y = 0.004 3X + 0.313 6; Y is the peak area ratio of the characteristic diffraction peak, X is the mass fraction of the trihydrate, the correlation coefficient r = 0.999 6; the precision of the method is 2.4%. The quantitative analysis of samples with 5.48%, 10.33% and 12.49% of trihydrate by standard curve showed that the absolute errors between measured and real values were 0.14%, 0.01% and 0.06%, respectively. Conclusion: The established method is accurate, reliable, rapid and simple and can be used for the quantitative analysis of the crystalline form of trihydrate and dihydrate Form A of esomeprazole magnesium.