摘要
以马来酸作为内标物质,氢核磁共振定量法(qHNMR)测定盐酸伊托必利片中盐酸伊托必利的含量。选择盐酸伊托必利δ7. 31~7. 40处为定量峰,马来酸δ6. 31处为内标峰,在恒温300K,弛豫延迟时间15 s,采样时间4. 01 s,扫描次数为64次条件下采集盐酸伊托必利片的qHNMR图谱。比较HPLC法与qHNMR法测定盐酸伊托必利片含量的结果。qHNMR法在2. 31~18. 66 mg·mL^-1的范围内线性关系良好。低、中、高浓度的平均回收率分别为98. 52%、99. 72%、101. 11%,RSD为1. 17%(n=9),检测限(LOD)为50. 0 ng·mL^-1,定量限(LOQ)为120. 0 ng·mL^-1。盐酸伊托必利片的qHNMR法含量测定结果与HPLC法的测定结果基本一致。qHNMR法可用于测定盐酸伊托必利片中盐酸伊托必利含量的测定。
Maleic acid was used as internal standard substance,the content of itopride hydrochloride tables was determined by quantitative proton nuclear magnetic resonance( qHNMR). Proton signal peaks at δ7. 31 ~ 7. 40 of itopride hydrochloride and δ6. 31 of maleic acid were served as quantitative peaks and internal standard peaks,respectively.The qHNMR spectra were collected at 300 K with 15 s relaxation delay,4. 01 s acquisition time and 64 scanning times.The determination results of HPLC and qHNMR were also been compared.There was a linear relationship for itopride hydrochloride in the range of 2. 31 ~ 18. 66 mg·mL^-1.The recoveries of low,middle and high concentration were 98. 52%,99. 72%and 101. 11%,and the average RSD was 1. 17%( n = 9). The limit of detection( LOD) was 50. 0 ng·mL^-1,and the limit of quantitation( LOQ) was 120. 0 ng·mL^-1. The content determination results of qHNMR method were generally consistent with those of HPLC method.The qHNMR could be used for the quantitative determination of itopride hydrochloride tablets..
作者
曹伶俐
杨宁辉
张智强
CAO Ling-li;YANG Ning-hui;ZHANG Zhi-qiang(Huanghe Science and Technology,Zhengzhou 45005,China;Henan Medical college,Xinzheng 451191,China;Tianjin Institute of Pharmaceutical Research Pharmaceutical Co.,Ltd,Tianjin 300301,China)
出处
《化学研究与应用》
CAS
CSCD
北大核心
2019年第8期1548-1551,共4页
Chemical Research and Application
基金
河南省科技厅重点研发与推广项目(18210231168)资助
