埃索美拉唑镁盐多晶型的X-射线粉末衍射定量分析

发布时间：2018-01-23 19:55

本文关键词： X-射线粉末衍射埃索美拉唑镁盐多晶型埃索美拉唑镁二水合物A晶型埃索美拉唑镁三水合物特征衍射峰定量分析标准曲线　出处：《药物分析杂志》2015年11期 　论文类型：期刊论文

【摘要】：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。
[Abstract]:Objective: to determine the content of crystal form in the mixture of esomeprazole magnesium trihydrate and dihydrate A by X-ray powder diffraction. To provide a feasible quantitative analysis method for the quality control of esomeprazole magnesium crystal type drug. The crystal form of esomeprazole magnesium trihydrate and the crystal form of dihydrate A were characterized by X-ray powder diffraction. The characteristic diffraction peak of esomeprazole magnesium trihydrate was 2 胃 ~ 5.27 掳. The ratio of the peak area to the characteristic diffraction peak of the crystal form A of dihydrate A (2 胃 ~ 5.65 掳I / I _ 0 ~ (100)) is a quantitative parameter. Set up the standard curve. The contents of crystal form of trihydrate and crystal form A of dihydrate in magnesium esomeprazole were determined. The area ratio of the characteristic diffraction peaks of esomeprazole magnesium dihydrate A crystal form and the characteristic diffraction peak of trihydrate has a good linear relationship with the content of trihydrate. In the range of 3 ~ 15% of hydrate content, the standard curve obtained is YT 0.004 3X 0.313 6; The peak area ratio X with Y as the characteristic diffraction peak is the mass fraction of gas trihydrate, and the correlation coefficient is 0.999 6. The precision was 2.4. The standard curve was used for quantitative analysis of the sample containing 5.48% and 10.33%. The results show that the absolute error between the measured value and the real value is 0.14%. Conclusion: the method is accurate, reliable, rapid and simple, and can be used for quantitative analysis of crystal form of trihydrate and crystal form A of dihydrate in magnesium esomeprazole.
【作者单位】：浙江中医药大学药学院;浙江大学化学系;
【基金】：浙江省分析测试科技计划项目(2014C37055)
【分类号】：R917
【正文快照】： 多晶型在有机固体药物中是一种非常普遍的现象。研究发现,药物的不同晶型常表现出不同的机械学、热力学、物理学和化学的特性,如可压缩性、熔点、溶解度和溶出速率等,从而影响药物的流动性、吸湿性、稳定性、制剂制备过程、生物利用度、药效及安全性等[1-2]。因此,药品在生产

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