氢核磁共振定量法测定盐酸伊托必利片含量

Quantitative nuclear magnetic resonance to determine the content of itopride hydrochloride tables

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..