核磁共振氢谱法定性和定量分析伐地那非  

Qualitative and quantitative analysis of vardenafil by ^(1)H NMR

作　　者：王瑾[1] 陈忠兰 朱雪坤 吴先富[1] 肖新月[1] WANG Jin;CHEN Zhong-lan;ZHU Xue-kun;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》2021年第7期1272-1276,共5页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立采用核磁共振氢谱(^(1)H NMR)对伐地那非进行定性和定量分析的方法。方法:将样品与经氢氧化钠碱化后的美国药典委员会(USP)对照品进行^(1)H NMR比对鉴别;采用Bruker AVANCE NEOAscend 600型核磁共振波谱仪,脉冲序列zg90,恒温25℃,驰豫延迟时间(D1)30 s。以1,3,5-三甲氧基苯为内标物,氘代二甲基亚砜(DMSO-d_(6))为溶剂,采用定量核磁共振氢谱法(qHNMR法)测定伐地那非的含量,同时含量测定结果与质量平衡法和外标法测定结果进行比较。结果:伐地那非样品的^(1)H NMR图谱和转化后的对照品的图谱一致;定量核磁共振氢谱法测得的伐地那非含量(99.8%)与质量平衡法(99.7%)、外标法(99.9%)测得结果一致。结论:NMR法可用于伐地那非定性鉴别和定量分析,简便准确。Objective:To establish a proton nuclear magnetic resonance(^(1)H NMR)method for the qualitative and quantitative study of vardenafil.Methods:The qualitative identification of vardenafil was based on the comparison of its ^(1)H NMR spectrum with that of USP reference standard after alkalization by sodium hydroxide.Quantitative ^(1)H NMR spectra were obtained in dimethylsulfoxide-d_(6)(DMSO-d_(6))with the internal standard 1,3,5-trimethoxybenzene by a Bruker AVANCE NEO 600 spectrometer.The parameters were set up as follows:zg90 for pulse sequence,30 s for the relaxation delay time,and the experiment temperature was controlled at 25℃.Meanwhile,the determination result was compared with those of mass balance method and external standard method.Results:The ^(1)H NMR spectra of vardenafil and reference standard after alkalization by sodium hydroxide were consistent.The content of vardenafil determinated by qHNMR was 99.8%,which was consistent with that by mass balance method(99.7%)and external standard method(99.9%).Conclusion:NMR method is simple and accurate for the qualitative identification and quantitative analysis of vardenafil.

关 键 词：伐地那非 核磁共振氢谱法 定性鉴别 含量测定 1 3 5-三甲氧基苯 

分 类 号：R917[医药卫生—药物分析学]