粉末X射线衍射技术定量分析左炔诺孕酮晶型

摘要

Objective According to the clinical medicinal crystal form———form γ of levonorgestrel, to establish the quantitative analysis method for levonorgestrel form γ by powder X-ray diffraction (PXRD) . Methods Firstly, single crystal X-ray diffractometry and powder X-ray diffractometry were used to confirm that the prepared levonorgestrel form γ was 100％ polymorphic purity, which provided a standard sample for quantitative analysis by single peak method; then, the standard samples of different quality levonorgestrel form γ for powder X-ray diffraction were weighed, the peak intensity values of characteristic diffraction peaks d = 6.4 , d = 6. 1  and d = 5. 6  of form γ as quantitative parameters selected, a linear relationship between the peak intensity value and the quality of form γ was established; finally, the content of levonorgestrel form γ was quantitatively analyzed. Results The peak intensity values of characteristic diffraction peaks d = 6.4 , d = 6.1  and d = 5.6  of levonorgestrel form γ and the quality showed a good linear relationship.In the range of form γ masses of 5 mg to 50 mg, the regression linear equations wereY = 459.59X+5 536.5, R2 = 0.993 0, Y = 430.03X+6 867.6, R2 = 0.990 5,Y = 615.95X+ 6 209.5, R2 = 0.990 8,respectively. Conclusion The method is simple, rapid, accurate and reliable, it can be used as quality control method for levonorgestrel polymorphs.%目的 针对紧急避孕药左炔诺孕酮的临床药用晶型物质———晶 γ 型,采用粉末 X 射线衍射法建立其原料药中晶 γ 型定量分析方法.方法 采用单晶 X 射线衍射法和粉末 X 射线衍射法确定了制备的左炔诺孕酮晶 γ 型为 100％晶型纯品,为单峰法定量分析提供标准样品.称取不同质量左炔诺孕酮晶 γ 型的标准样品进行粉末 X 射线衍射实验,选择晶 γ 型的特征衍射峰 d = 6.4、 d = 6.1 和 d = 5.6 的峰强度值为定量参数,建立峰强度值与晶型质量间的线性关系,用于定量分析左炔诺孕酮原料药中晶 γ 型的含量.结果 左炔诺孕酮晶 γ 型中 3 个(d = 6.4、 d = 6.1 和 d = 5.6) 特征衍射峰的峰强度值与晶 γ 型的质量呈良好的线性关系; 在晶 γ 型质量为 5～ 50 mg 内,回归线性方程分别为Y = 459.59X +5 536.5,R2 = 0.993 0、 Y = 430.03 X +6 867.6,R2 = 0.990 5 和 Y = 615.95 X +6 209.5,R2 = 0.990 8.结论 该方法操作简单便捷,定量分析准确可靠,可作为左炔诺孕酮原料药的晶型质量控制方法.