定量核磁共振氢谱法测定甲磺酸奥希替尼的含量  

Determination of osimertinib mesylate by quantitative proton nuclear magnetic resonance

作　　者：王瑾[1] 陈忠兰 冯玉飞[1] 吴先富[1] 肖新月[1] WANG Jin;CHEN Zhong-lan;FENG Yu-fei;WU Xian-fu;XIAO Xin-yue(National Institutes for Food and Drug Control,Beijing 102629,China)

机构地区：[1]中国食品药品检定研究院,北京102629

出　　处：《药物分析杂志》2020年第8期1510-1513,共4页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立定量核磁共振氢谱法(qHNMR)测定甲磺酸奥希替尼的含量。方法:采用Bruker Ascend600型核磁共振波谱仪测定核磁共振氢谱,90°脉冲,弛豫延迟时间(D1)30 s,扫描次数(NS)32次,测定温度298.0 K,以对苯二甲酸二甲酯(DMT)为内标,氘代二甲亚砜(DMSO-d6)为溶剂,对甲磺酸奥希替尼进行定量研究。结果:测得甲磺酸奥希替尼以奥希替尼计含量为82.03%(RSD=0.49%,n=6),与质量平衡法测定结果(82.03%)一致。结论:该法操作简单、准确,可用于甲磺酸奥希替尼的含量测定。)Objective:To establish a method for the determination of osimertinib mesylate by quantitative proton nuclear magnetic resonance(qHNMR). Methods:The qHNMR spectra were obtained in dimethylsulfoxide-d6(DMSO-d6) with the internal standard dimethyl erephthalate(DMT) by a Bruker Ascend 600 spectrometer. The parameters of which were set up as follows:90° pulse sequences,the relaxation delay time was 30 s,the number for scanning was 32,and the experiment temperature was controlled at 298 K. Results:The content of osimertinib mesylate determinated by qHNMR was 82.03%(RSD=0.49%,n=6),which was consistent with that by mass balance mehtod(82.03%). Conclusion:The estabilised qHNMR method is simple and accurate for the determination of osimertinib mesylate.

关 键 词：定量核磁共振氢谱法 含量测定 甲磺酸奥希替尼 对苯二甲酸二甲酯(DMT) 质量平衡法 

分 类 号：R917[医药卫生—药物分析学]