Yi Tao, Zhang Hao, Cai Zongwei
West China School of Pharmacy, Sichuan University, No. 17 Section 3 Ren-Min-Nan-Lu Road, Chengdu, Sichuan 610041, People's Republic of China.
Phytochem Anal. 2007 Sep-Oct;18(5):387-92. doi: 10.1002/pca.993.
An HPLC method with photodiode array detection (PAD) and ESI/MS detection was developed for the qualitative and quantitative analysis of the major chemical constituents of the dried rhizome of Polygonum cuspidatum Sieb. et Zucc. (Rhizoma Polygoni Cuspidati; Chinese name Hu-Zhang). Based on the chromatographic separation on an Altima C(18) column using 0.5% aqueous acetic acid and acetonitrile as the mobile phase, nine compounds, including stilbenes, stilbene glucosides, anthraquinones and anthraquinone glucosides, were identified by online ESI/MS analysis and seven were quantified by HPLC-PAD. A full validation of the method including sensitivity, linearity, repeatability and recovery was conducted. Linear calibration was achieved over the concentration range 1-200 mg/L with R(2) > 0.999, whilst the limits of detection ranged from 0.51 to 1.57 ng. Repeatability was evaluated by intra- and inter-day assays and the RSD value was within 1.79%. Recoveries of the quantified compounds were within the range 96.0-100.1% with RSD values of less than 2.2%. Five samples of Rhizoma Polygoni Cuspidati from different regions were analysed using the developed method. The major constituents piceid, resveratrol, emodin-8-O-beta-D-glucoside and emodin were selected to provide an index for the quality assessment of the herbal drug.
建立了一种采用光电二极管阵列检测（PAD）和电喷雾电离/质谱检测（ESI/MS）的高效液相色谱法，用于虎杖干燥根茎（虎杖；中药名虎杖）主要化学成分的定性和定量分析。基于在Altima C(18)柱上以0.5%乙酸水溶液和乙腈为流动相进行色谱分离，通过在线ESI/MS分析鉴定了9种化合物，包括芪类、芪糖苷、蒽醌类和蒽醌糖苷类，其中7种通过HPLC-PAD进行定量。对该方法进行了全面验证，包括灵敏度、线性、重复性和回收率。在1-200 mg/L的浓度范围内实现了线性校准，R(2) > 0.999，而检测限范围为0.51至1.57 ng。通过日内和日间测定评估重复性，相对标准偏差（RSD）值在1.79%以内。定量化合物的回收率在96.0-100.1%范围内，RSD值小于2.2%。采用所建立的方法对来自不同地区的5个虎杖样品进行了分析。选择主要成分白藜芦醇、白藜芦醇、大黄素-8-O-β-D-葡萄糖苷和大黄素作为该草药质量评估的指标。
