粉末X射线衍射法测定甘氨酸原料药中α晶型的含量

Determination of Crystal Type α in Glycine by Powder X-ray Diffraction

目的:应用粉末X-射线衍射法对甘氨酸原料药中α晶型的含量进行定量分析,为多晶型研究提供实验依据。方法:分别选择α晶型的特征衍射峰2θ=19. 1°与γ晶型特征衍射峰2θ=25. 4°的峰强度比值为定量参数,建立标准曲线,测定α晶型的含量。结果:获得甘氨酸α晶型与γ晶型的表征图谱,α晶型的线性范围为1%～99%(r=0. 996 7),平均回收率为102. 8%(RSD=4. 0%,n=9)。结论:所建方法准确可靠,快速简便,可用于甘氨酸原料药中α晶型的定量分析。

Objective： To determine the content of crystal type α in glycine by X-ray power diffraction technique to provide evidence for the polymorphic research. Methods： A calibration curve was established by using the characteristic peak ratio of glycine formα at 2θ = 19. 1° to form γ at 2θ = 25. 4° as the quantitative parameter to determine the content of crystal type α. Results： The characterization figures of form α and form γ were obtained. The linear range of form α was 1%-99%（ r = 0. 996 7）,and the average recovery was 102. 8% with the RSD of 4. 0%（ n = 9）. Conclusion： X-ray powder diffraction method is a feasible analytical method for the quantitative determination of form α and form γ of glycine with simple,sensitive and accurate properties.