风芍六君子汤水煎液HPLC指纹图谱研究

目的: 采用HPLC 法建立风芍六君子汤水煎液的指纹图谱,并对其主要的指标性成分没食子酸、芍药苷和橙皮苷进行含量测定,为其成分结构分析和质量控制提供研究基础。方法: 采用Diamonsil 钻石C₁₈(250 mm×4.6 mm,5 μm)色谱柱,以乙腈-0.2% 磷酸水溶液为流动相,梯度洗脱(0~6 min,5%A;6~12min,5%A→15%A;12~35 min,15%A→35%A;35~40 min,35%A→55%A;40~65 min,55%A→75%A;65~80 min,75%A→100%A;80~85 min,100%A),流速1.0 mL·min^-1,柱温35 ℃,检测波长230 nm,采用《中药色谱指纹图谱相似度评价系统软件(2004A 版)》,确定共有峰,计算相似度,并对其色谱峰进行了指认和归属。结果: 建立了风芍六君子汤水煎液的指纹图谱,并对其方法学进行了验证,确定了指纹图谱中的19 个共有峰,其相似度大于0.95,共有峰的相对保留时间及相对峰面积的RSD 均小于3%,归属了其中的18 个峰,并指认了没食子酸、对羟基苯甲醛等10 个色谱峰的化学结构;没食子酸、芍药苷、橙皮苷的含量分别为3.819、9.053 和6.558 mg·g^-1。结论: 风芍六君子汤水煎液HPLC 指纹图谱的精密度、稳定性和重复性良好,峰的指认归属准确,能够有效的控制其质量。

Objective: To explore the fingerprints of Fengshao Liujunzi decoction and determine the content of some main key materials,such as gallic-acidgallic acid,peoniflorin and hesperidin by HPLC,and provide a research basis for drug quality control. Methods: A Diamonsi C₁₈(250 mm×4.6 mm,5 μm)column was adopted with acetonitrile-0.2% phosphate aqueous as the mobile phase by gradient elution. Namely,0-6 min,5%A;6-12 min, 5%A→15%A;12-35 min,15%A→35%A;35-40 min,35%A→55%A;40-65 min,55%A→75%A;65-80 min,75%A→100%A;80-85 min,100%A. The flow rate was 1.0 mL·min^-1,the temperature of column was 35 ℃,and the detective wavelength was 230 nm. Chromatographic fingerprint evaluation system software(2004A Edition)was used to determine the common peaks. The similarity was calculated,and its chromatographic peaks were identified and attributed. Results: The fingerprints of Fengshao Liujunzi decoction were established and the methods were verified. Nineteen common peaks of the fingerprints were determined,and their similarity was greater than 0.95,RSD of retention time and relative peak area was no more than 3%,in which 18 peaks belonged to the common peaks,and the chemical structures of 10 peaks were identified,including gallic-acidgallic acid and parahydroxyben-zaldehyde. The content of gallic-acidgallic acid,peoniflorin and hesperidin were 3.819,9.053 and 6.558 mg·g^-1,respectively. Conclusion: HPLC fingerprint of the Decoction exhibits nice precision,stability and reproducibility. The identification and attribution of 18 peaks are accurate,which can be applied to the quality control.