NMPA Key Laboratory for Core Technology of Generic Drug Evaluation, Zhejiang Institute for Food and Drug Control, Hangzhou 310052, China.
Zhejiang University of Technology, Hangzhou 310014, China.
J AOAC Int. 2021 Jun 12;104(3):579-584. doi: 10.1093/jaoacint/qsaa166.
Losartan potassium, a common antihypertensive drug on the market, has multiple polymorphs, of which form I is used as a pharmaceutical crystal form. Form I can be partially converted to form III under some circumstances. The quantification of losartan potassium polymorphs is important to control the quality of pharmaceuticals.
To establish a method to determine the contents of losartan potassium polymorphs.
Pure form I and form III of losartan potassium were obtained by recrystallization, and characterized by powder X-ray diffraction (PXRD), Fourier transform infrared spectroscopy, Raman spectroscopy, and thermal analysis. A powder X-ray diffraction method was developed to characterize form I and form III of losartan potassium. Peak area and weight percentage were used to establish calibration curve.
The calibration curve was linear over the range of 1-50% (w/w), using the characteristic peak area ratio of form I at 11.13° 2θ and form III at 5.64° 2θ as the quantitative parameter. The precisions were excellent between 0.6-4.9%, and the limit of quantification was 2.02% (w/w).
This PXRD method can be used to analyze mixtures of losartan potassium polymorphs (forms I and III) quantitatively and control the quality of bulk drug.
This is a new method of quantifying the amount of form III in polymorphic forms of losartan potassium using data obtained by PXRD. It is consistent, sensitive, and accurate.
市场上常见的降压药氯沙坦钾有多晶型，其中晶型 I 被用作药用晶型。在某些情况下，晶型 I 可以部分转化为晶型 III。定量分析氯沙坦钾多晶型物对于控制药品质量非常重要。
建立一种测定氯沙坦钾多晶型物含量的方法。
通过重结晶获得纯的氯沙坦钾晶型 I 和晶型 III，并通过粉末 X 射线衍射（PXRD）、傅里叶变换红外光谱、拉曼光谱和热分析对其进行表征。建立了一种粉末 X 射线衍射法来表征氯沙坦钾的晶型 I 和晶型 III。采用峰面积和重量百分比建立校准曲线。
校准曲线在 1-50%（w/w）范围内呈线性，以晶型 I 在 11.13° 2θ 和晶型 III 在 5.64° 2θ 的特征峰面积比作为定量参数。精密度在 0.6-4.9%之间非常好，定量限为 2.02%（w/w）。
该 PXRD 方法可用于定量分析氯沙坦钾多晶型物（晶型 I 和晶型 III）混合物，并控制原料药的质量。
这是一种使用 PXRD 获得的数据定量测定氯沙坦钾多晶型物中晶型 III 含量的新方法。该方法具有一致性、灵敏度和准确性。
