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中国药学(英文版) ›› 2015, Vol. 24 ›› Issue (3): 177-184.DOI: 10.5246/jcps.2015.03.022

• 【研究论文】 • 上一篇    下一篇

改进的校正标准分离度积评价大豆异黄酮提取物高效液相指纹图谱

沈卫阳1,2*, 卞娟1,2, 刘斐烨1,2, 彭水芳1,2   

  1. 1. 药物质量与安全预警教育部重点实验室, 江苏 南京 210009
    2. 中国药科大学理学院 分析化学教研室, 江苏 南京 210009
  • 收稿日期:2014-10-01 修回日期:2014-12-18 出版日期:2015-03-29 发布日期:2014-12-29
  • 通讯作者: Tel.:18061297399
  • 基金资助:
    National Higher-Education Institution General Research and Development Funding (Grant No. JKP2011010).

An improved calibrated normalized resolution product (r*') and the application in HPLC fingerprints of soy isoflavone extract

Weiyang Shen1,2*, Juan Bian1,2, Feiye Liu1,2, Shuifang Peng1,2   

  1. 1. Key Laboratory of Drug Quality Control and Pharmacovigilance, Ministry of Education, Nanjing 210009, China
    2. Department of Analytical Chemistry, China Pharmaceutical University, Nanjing 210009, China
  • Received:2014-10-01 Revised:2014-12-18 Online:2015-03-29 Published:2014-12-29
  • Contact: Tel.:18061297399
  • Supported by:
    National Higher-Education Institution General Research and Development Funding (Grant No. JKP2011010).

摘要:

本文提出了一种新的评价色谱指纹图谱分离质量的指标, 即改进的校正标准分离度积(ri*')。以大豆异黄酮提取物为分析对象, 通过正交设计对高效液相梯度洗脱的初始甲醇比例、洗脱结束时的甲醇比例以及洗脱时间进行考察,改进的校正标准分离度积(ri*')衡量所得色谱图, 通过与校正标准分离度积(ri*)及谱系色谱响应函数(HCRF)进行比较,分析各个指标的优缺点, 论证了改进的校正标准分离度积(ri*')这一评估指标的有效性, 并建立了大豆异黄酮提取物指图谱的优化色谱条件(流动相A: 0.1%醋酸, B: 甲醇; 梯度洗脱B; 流速: 1.0 mL/min检测波长: 254 nm;柱温: 36 ºC)。此外, 高效液相色谱-电喷雾质谱法对大豆异黄酮提取物的活性成分进行了归属分析。

关键词: 改进的校正标准分离度积, 指纹图谱, 大豆异黄酮, 高效液相色谱-电喷雾质谱法

Abstract:

In this paper, we proposed a novel resolution criterion (improved calibrated normalized resolution product, r*') to evaluate separation quality of fingerprints. By comparing with the calibrated normalized resolution product (r*) and the hierarchical chromatographic response function (HCRF), the validity of this criterion was demonstrated by experimental chromatograms. The soy isoflavone extract was selected as the analytical object. The initial and end percentages of methanol and elution time affectinggradient elution were tested by orthogonal design. The final optimized conditions were as follows. It was detected by UV absorbance at 254 nm, column temperature was maintained at 36 ºC, solvent A was 0.1% (v/v) acetic acid, solvent B was methanol, gradient elution was from 34% to 65% B in a linear gradient in 25 min, and the flow-rate was set at 1.0 mL/min. In addition, the main ingredients of the soy isoflavone extract were confirmed by LC-ESI/MS.

Key words: Improved calibrated normalized resolution product, Fingerprints, Soy isoflavones, LC-ESI/MS

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