定量核磁共振波谱法测定白芷中欧前胡素含量

Determination of imperatorin in Angelica dahuricae by quantitative nuclear magnetic resonance(qNMR)spectroscopy

为建立定量核磁共振波谱法测定白芷中欧前胡素含量的方法,以对苯二酚为内标、氘代二甲基亚砜(DMSO-d6)为溶剂,在400 MHz光谱仪上进行了qNMR测量。选择测定温度为293.7 K,谱宽(SWH)为8012.8 Hz,采样时间(AQ)为4.0 s,弛豫时间(D1)为1 s,脉冲宽度(P1)14.90 s,扫描次数(NS)为32次,空扫次数(DS)为2次,以欧前胡素中δ7.65的峰为定量峰,对苯二酚中δ6.55的峰为内标定量峰。对线性关系、检测限、定量限、精密度、重复性、稳定性和回收率等进行了方法学评价,结果良好。采用高效液相色谱法加以验证,2种方法测定结果基本一致,表明qNMR可用于白芷中欧前胡素含量测定。

A quantitative nuclear magnetic resonance(qNMR)spectroscopy for determining the imperatorin content in traditional Chinese medicine Angelica dahuricae was established.The qNMR measurements were performed on 400 MHz spectrometer with hydroquinone as the internal standard reference in deuterated dimethyl sulfoxide(DMSO-d6)solvent.The temperature was 293.7 K,spectral width(SWH)was 8012.8 Hz,sampling time(AQ)was 4.0 s,relaxation time(D1)was 1 s,pulse width(P)was 14.90 s,the number of scans(NS)was 32 times,the number of empty sweep(DS)was two times.The peak ofδ7.65 in imperatorin and the peck ofδ6.55 in hydroquinone were selected as quantitative peak and internal standard peak,respectively.The linearity,detection limit,the limit of quantification,precision,reproducibility,stability and recovery were evaluated by methodology,and results were good.The obtained results were validated by high performance liquid chromatography(HPLC)method.The determined contents of imperatorin by qNMR are in accordance with the results by HPLC,indicating that qNMR can be applied to determine imperatorin of Angelica dahuricae.