定量核磁共振波谱法同时测定中药虎杖中白藜芦醇和虎杖苷的含量  

Simultaneous Determination of Resveratrol and Polydatin in Polygonum Cuspidatum by Quantitative Nuclear Magnetic Resonance Spectroscopy

作　　者：禹珊 郭强胜[1] 王会琳[2] 高建平[2] 许旭[1,3] 

机构地区：[1]上海应用技术学院化学与环境工程学院,上海201418 [2]上海中医药大学中药学院,上海201203 [3]中国科学院天然产物有机合成化学重点实验室,上海200032

出　　处：《分析化学》2015年第1期69-74,共6页Chinese Journal of Analytical Chemistry

基　　金：中国科学院天然产物有机合成化学重点实验室研究基金资助项目(2013-2014)

摘　　要：建立了定量核磁共振波谱法同时测定虎杖中白藜芦醇和虎杖苷的方法。样品用80%乙醇和丙酮两次超声提取净化,再用定量核磁共振波谱法测定。考察了样品预处理和核磁共振实验条件对测定结果的影响,选择氘代二甲亚砜-重水（10∶1,V/V）为溶剂,用基准物质邻苯二甲酸氢钾标定的2,3,5-三碘苯甲酸为内标,选择脉冲延迟时间为5 s,采样次数为32次。定量峰为6.388～6.391（白藜芦醇：H-2,6,d,2H）和6.322～6.330（虎杖苷：H-4,t,1H）。结果表明,NMR测定的精密度均小于0.6%,线性相关系数（r）均大于0.999,白藜芦醇和虎杖苷的检出限分别为0.23和0.24 g/L,定量限分别为0.69和1.57 g/L,包括样品提取过程的回收率分别为97.7%～103.5%（RSD=2.4%）和94.5%～99.2%（RSD=1.6%）,显示出定量核磁共振法在中药定量时的可靠性。实际测定4种虎杖饮片及配方颗粒样品中白藜芦醇和虎杖苷含量分别为3.57～5.69 mg/g和12.73～24.07 mg/g。A quantitative nuclear magnetic resonance spectroscopic（ q NMR） method was established for the simultaneous determination of resveratrol and polydatin in Polygonum Cuspidatum traditional Chinese herb cuts and granule. The 2-step ultrasonic extraction method using 80% alcohol and acetone was used for fully extracting these two components in samples before q NMR determination. The q NMR experimental conditions were investigated and deuterated dimethyl sulphoxide-deuterium oxide（ 10∶ 1,V / V） was selected as solvent,the pulse delay time was 5 s,the scan number was 32,2,3,5-triiodobenzoate was used as internal standard which was calibrated with primary standard substance of potassium hydrogen phthalate. The ^1H-NMR peaks atδ 6. 388- 6. 391（ d,2H） of resveratrol and δ 6. 322- 6. 330（ t,1H） of polydatin were chosen as the quantitative peaks. Method validation was performed in terms of precision（ RSD 〈0. 6%）, linearity（ correlative constants R^2〉 0. 999）,limit of detection（ 0. 23 g / L for resveratrol and 0. 24 g / L for polydatin）and limit of quantitation（ resveratrol 0. 69 g / L,polydatin 1. 57 g / L）,recovery（ resveratrol 97. 7%-103. 5%,RSD = 2. 4%,polydatin 94. 5%- 99. 2%,RSD = 1. 6%,including the sample extraction and preparaton process）. The results showed the reliability of q NMR for traditional Chinese medicine assay. The resveratrol and polydatin in Polygonum Cuspidatum real cuts and granule samples were experimental determined as 3. 57- 5. 69 mg / g and 12. 73- 24. 07 mg / g,respectively.

关 键 词：定量核磁共振 虎杖 白藜芦醇 虎杖苷 

分 类 号：O657.2[理学—分析化学] R286.0[理学—化学]