运用X射线粉末衍射法测定甲磺酸仑伐替尼胶囊中晶型C含量  

Determination of the Content of Form C in Lenvatinib Mesylate Capsules byX-ray Powder Diffraction

作　　者：李宗栋 申建伟 赵金红 吴晶 柴雨柱 LI Zongdong;SHEN Jianwei;ZHAO Jinhong;WU Jing;CHAI Yuzhu(Nanjing Chai Tai Tianqing Pharmaceutical Co.,Ltd.,Nanjing 210046,China)

机构地区：[1]南京正大天晴制药有限公司,江苏南京210046

出　　处：《山东化工》2025年第7期165-167,共3页Shandong Chemical Industry

摘　　要：目的:通过开发X射线粉末衍射法(XRPD)来检测甲磺酸仑伐替尼胶囊中晶型C的含量。方法:使用铜靶石墨单色器;设置管路电压40 kV、管路电流40 mA;探测器为LynxEye以及探测狭缝设置为5 mm;扫描范围:5°~11°,扫描速度:12 s/step,扫描步长:0.02(°)/step。结果:在6.1°±0.2°(2θ)处甲磺酸仑伐替尼无定型样品和处方比例的空白辅料均对甲磺酸仑伐替尼晶型C的检测无干扰,在含晶型C(以仑伐替尼计)0.5%~8%范围内线性关系良好,r为0.998,定量限为0.5%,准确度考察结果RSD为5.4%(n=6)。结论:专属性、精密度以及准确度均良好,可应用于甲磺酸仑伐替尼胶囊中晶型C的定量检测。Objective:To develop an X-ray powder diffraction(XRPD)method for the detection of the content of crystalline form C in lenvatinib mesylate capsules.Method:A copper target graphite monochromator was used.The tube voltage was set to 40 kV and the tube current to 40 mA.The detector was LynxEye with a detection slit set to 5 mm.The scanning range was 5°to 11°,the scanning speed was 12 s/step,and the scanning step size was 0.02(°)/step.Results:At 6.1°±0.2°(2θ),both the amorphous sample of lenvatinib mesylate and the blank excipients in the prescription ratio did not interfere with the detection of crystalline form C of lenvatinib mesylate.A good linear relationship was observed in the range of 0.5%to 8%of crystalline form C(calculated as lenvatinib),with a correlation coefficient r of 0.998,and the quantitation limit was 0.5%.The accuracy assessment resulted in an RSD of 5.4%(n=6).Conclusion:The specificity,precision,and accuracy are all good,and it can be applied to the quantitative detection of crystalline form C in lenvatinib mesylate capsules.

关 键 词：甲磺酸仑伐替尼胶囊 X射线粉末衍射 晶型C 定量 

分 类 号：O657.3[理学—分析化学]