独脚金药材HPLC-DAD特征图谱研究

目的：建立独脚金药材的HPLC-DAD特征图谱。方法：采用HPLC法测定，使用Acchrom XAqua C18色谱柱（4.6 mm×250 mm，5 μm），以乙腈-0.1% 磷酸水溶液为流动相，梯度洗脱，流速1 mL·min^-1，检测波长为340 nm，柱温为30 ℃。对10 个批次独脚金药材检测，采用国家药典委员会中药色谱指纹图谱相似度评价系统软件（2008 版）进行数据处理分析。并用HPLC-ESI-MS 技术对部分共有峰进行了初步归属。结果：建立了以8个共有峰为指标成分的独脚金药材HPLC 特征图谱，并通过MS 技术初步鉴定出7 个共有峰的可能化学成分，分别为木犀草素-7-O-β-D-葡萄糖醛酸苷（2号峰）、芹菜素-7- 半乳糖醛酸苷或芹菜素-7-O-β-D-吡喃葡萄糖醛酸苷（3号峰）、金圣草素-7-O-β-D-葡萄糖醛酸苷（4号峰）、木犀草素（5号峰）、刺槐素-7-O-β-D-葡萄糖醛酸苷（6号峰）、芹菜素（7号峰）、金圣草素（8号峰）。以木犀草素色谱峰为参照，其他7 个色谱峰的相对保留时间分别为（0.441±0.004）、（0.513±0.004）、（0.665±0.010）、（0.727±0.005）、（1.048±0.005）、（1.258±0.008）、（1.333±0.009）。结论：该方法经过方法学验证，可用于独脚金药材的质量控制。

Objective:To establish the characteristic chromatogram of whole herb of Striga asiatica by HPLCDAD. Methods:The analysis was performed on an Acchrom XAqua C18 column(4.6 mm×250 mm,5 μm)with gradient mobile phase of acetonitrile-0.1% phosphoric acid aq.at a flow rate of 1 mL·min^-1.The detection wavelength was set at 340 nm,and the column temperature was 30 ℃.Ten batches of samples of whole herb of S.asiatica were analyzed with the established method,and similarity evaluation system for chromatographic fingerprint of traditional Chinese medicine(2008 Version)was used for the quality assessment.Some characteristic peaks were identified preliminarily based on the MS spectra and literature data.Results:Eight common peaks were found through the similarity evaluation system.Seven peaks,including luteolin-7-O-β-D-glucuronide(peak No.2),apigenin- 7-galacturonide or apigenin-7-O-β-D-glucopyranuronide(peak No.3),chrysoeriol -7-O-β-D-glucuronide (peak No.4),luteolin(peak No.5),acacetin-7-O-β-D-glucuronide(peak No.6),apigenin(peak No.7), chrysoeriol(peak No.8)were identified by comparison of the retention time and MS data with those of reference substances and reported in reference.With luteolin peak as the reference,the relative retention time of the other seven peaks were(0.441±0.004),(0.513±0.004),(0.665±0.010),(0.727±0.005),(1.048±0.005), (1.258±0.008),and(1.333±0.009),respectively.Conclusion:The developed method conforms to the requirements of methodology validation,which can be used for the quality control of whole herb of S.asiatica.