定量核磁共振波谱法测定气滞胃痛颗粒中芍药总苷与其苷元的总量  

qNMR Determination of Total Amount of Total Glucosides of Paeony and Their Aglycones in Qizhiweitong Granules

作　　者：鞠钰蕊 赵玥祯 肖坤 郭强胜 许旭 JU Yurui;ZHAO Yuezhen;XIAO Kun;GUO Qiangsheng;XU Xu(School of Chemical and Environmental Engineering,Shanghai Institute of Technology,Shanghai 201418,China)

机构地区：[1]上海应用技术大学化学与环境工程学院,上海201418

出　　处：《理化检验（化学分册）》2020年第12期1245-1253,共9页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：国家自然科学基金面上项目(31671928);上海市自然科学基金(15ZR1440800)。

摘　　要：以氘代二甲基亚砜为氘代试剂,以2,3,5-三碘苯甲酸为内标,采用定量核磁共振波谱法测定气滞胃痛颗粒中芍药总苷与其苷元的总量(以芍药苷计)。脉冲宽度为14.1μs,延迟时间为1 s,扫描次数为256,芍药苷的定量峰为H-2″,6″(δ 7.84~7.93)。芍药苷的线性范围为0.555 3~1.102 mg,检出限为1.0 mg·L^(-1),测定下限为3.5 mg·L^(-1)。方法用于气滞胃痛颗粒样品的分析,测定值的日内相对标准偏差(n=6)为0.83%,日间相对标准偏差(n=6)为0.92%,加标回收率为95.9%~99.7%。Deuterated dimethyl sulfoxide and 2,3,5-triiodobenzoic acid were used as deuterated reagent and internal standard respectively. qNMR was applied to the determination of total amount of total glucosides of paeony and their aglycones(calculated by paeoniflorin) in Qizhiweitong granules. The pulse width was 14.1 μs, the delay time was 1 s, and the scan number was 256. The quantitative peak of paeoniflorin was H-2″,6″(δ 7.84-7.93). Linearity range of paeoniflorin was found in the range of 0.555 3-1.102 mg, with detection limit of 1.0 mg·L^(-1) and lower limit of determination of 3.5 mg·L^(-1). The proposed method was applied to the analysis of the sample of Qizhiweitong granules, giving values of intra-day RSD(n=6) and inter-day RSD(n=6) of determined values of 0.83% and 0.92% respectively, and values of recovery found by standard addition method in the range of 95.9%-99.7%.

关 键 词：定量核磁共振波谱法 芍药苷 芍药总苷 芍药苷元 气滞胃痛颗粒 

分 类 号：O657.2[理学—分析化学]