吉非替尼的两种核磁共振定量方法  

Determination of Gefitinib by Two Methods of Quantitative Nuclear Magnetic Resonance

作　　者：郝海军[1] 贾幼智[1] 韩茹[1] 胡彬[1] 

机构地区：[1]中国医药工业研究总院上海医药工业研究院,上海201203

出　　处：《中国医药工业杂志》2017年第5期711-715,共5页Chinese Journal of Pharmaceuticals

摘　　要：分别采用氢核磁共振定量法和氟核磁共振定量法测定吉非替尼含量。氢核磁共振定量法以化学位移δ7.21为定量峰,马来酸δ6.02为内标峰,在测试温度300 K,谱宽8 012 Hz,采样时间4.01 s,弛豫延迟时间20 s,脉冲宽度9.54μs,扫描次数64次条件下采集氢谱。氟核磁共振定量法以4-溴-2-氟乙酰苯胺为内标,脉冲序列zgfhigqn.2在恒温300 K下采集氟谱。两种核磁定量方法都进行了方法学验证。吉非替尼氢核磁共振定量法和氟核磁共振定量法含量测定结果与质量平衡法结果基本一致。本研究建立的核磁共振定量方法专属性强、快速、准确,可用于吉非替尼的含量测定。Proton nuclear magnetic resonance （^1H NMR） and fluorine nuclear magnetic resonance （^19F NMR） were employed for the determination of gefitinib. ^1H NMR spectra were collected at 300 K with a 8 012 Hz spectral width, 4.01 s acquisition time, 20 s relaxation delay, 9.54 9s pulse width and 64 scanning times. ^19F NMR spectra were obtained by zgfhigqn.2 pulse sequence at 300 K with the internal standard of 4-bromo-2-fluoroacetanilide. Their methodologies were validated. The results of both ^1H NMR and ^19F NMR were generally consistent with that of the mass balance method. The established methods were specific, rapid and accurate, and were suitable for the quantitative determination of gefitinib.

关 键 词：吉非替尼 氢核磁共振定量法 氟核磁共振定量法 含量测定 

分 类 号：O657.61[理学—分析化学] TQ460.72[理学—化学]