1^H定量核磁共振内标法测定磷酸奥司他韦原料药含量

Content Determination of Oseltamivir Phosphate by ~1H qNMR

目的:建立一种~1H定量核磁共振内标法以测定磷酸奥司他韦原料药含量。方法:采用Bruker400MHz核磁共振波谱仪,以氘代DMSO为溶剂,苯甲酸苄酯为内标,O1Pδ4.26,弛豫时间20 s,扫描次数32次的条件下,使用zg30脉冲序列磷酸奥司他韦原料药的氢谱。以化学位移值δ5.38的苯甲酸苄酯峰和化学位移值δ3.13~3.20的磷酸奥司他韦峰作为定量峰,两者的峰面积比对质量比在测定的质量浓度范围线性关系良好;核磁共振内标法测得磷酸奥司他韦原料药含量为95.80%,质量平衡法测得磷酸奥司他韦原料药含量为96.79%,二者结果吻合。结论:1H定量核磁共振内标法简便、准确,可用于磷酸奥司他韦的含量测定,同时可作为质量平衡法结果的有力佐证。

Objective:A method for the content determination of oseltamivir phosphate by ~1 H qNMR.Methods:~1 H NMR were obtained in DMSO-d6,with the internal standard benzyl benzoate,O1 P δ4.26,relaxation delay time 20 s,number of scan 32,and zg30 pulse sequence by using a Bruker AVANCE Ⅲ 400 MHz spectrometer.~1 H NMR peak at δ5.36 of benzyl benzoate and δ3.13~3.20 of oseltamivir phosphate were used as quantitative peaks.The linear relationship of the corresponding peak area ratio is good in the concentration range under investigation.The content of oseltamivir phosphate determined by ~1 H qNMR was 95.80 %.The content of oseltamivir phosphate determined by mass balance method was 96.79 %.The results are consistent.Conclusion:~1 H qNMR is simple and rapid,can be applied to content determination of oseltamivir phosphate,and used as a strong evidence for the results of mass balance method.