色谱

色谱 ›› 2013, Vol. 31 ›› Issue (8): 753-757.DOI: 10.3724/SP.J.1123.2013.01018

• 研究论文 • 上一篇    下一篇

梯度液相色谱保留时间公式在梯形梯度洗脱研究中的应用

孙小丽1, 郝卫强2, 王俊德3, 狄斌4, 陈强2, 庄韦2, 俞强1, 张培培1   

  1. 1. 常州大学材料科学与工程学院, 江苏 常州 213164;
    2. 常州南京大学高新技术研究院, 江苏 常州 213164;
    3. 中国科学院大连化学物理研究所, 辽宁 大连 116023;
    4. 中国药科大学药物分析教研室, 江苏 南京 210009
  • 收稿日期:2013-01-08 修回日期:2013-02-06 出版日期:2013-08-28 发布日期:2013-09-29
  • 通讯作者: 郝卫强
  • 基金资助:

    国家自然科学基金项目(21005009,81173022);常州市应用基础研究计划(CJ20115002).

Application of general retention time formula for gradient liquid chromatography in the studies of ladder-like gradient elution

SUN Xiaoli1, HAO Weiqiang2, WANG Junde3, DI Bin4, CHEN Qiang2, ZHUANG Wei2, YU Qiang1, ZHANG Peipei1   

  1. 1. School of Materials Science and Engineering, Changzhou University, Changzhou 213164, China;
    2. Changzhou High-Tech Research Institute of Nanjing University, Changzhou 213164, China;
    3. Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China;
    4. Department of Pharmaceutical Analysis, China Pharmaceutical University, Nanjing 210009, China
  • Received:2013-01-08 Revised:2013-02-06 Online:2013-08-28 Published:2013-09-29
  • Contact: O658

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227

被引次数

3

摘要：

根据前期得到的梯度液相色谱保留时间计算公式,在不指定溶剂强度模型形式的前提下,探讨了梯形梯度洗脱的一些特点。对于溶质在梯形梯度坡度上流出时的情形,推导得到溶质流出色谱柱所对应的流动相组成(φR)随梯度斜率(B)变化的表达式。该公式表明,在该情形中φR将会随着B值的增加而增加。对于溶质在梯形梯度最后一个等度区间流出时的情形,如果初始和终止流动相组成保持不变而仅有梯度的斜率发生变化时,从理论上证明了溶质保留时间(tR)与梯度斜率的倒数(1/B)之间呈线性关系。实验中以C18色谱柱为固定相,甲醇-水为流动相,联苯为样品,测定了不同流动相组成以及梯形梯度条件下的保留时间,所得到的实验值与理论值吻合,从而验证了理论方法的正确性。

关键词: 保留值, 梯度洗脱, 梯形梯度, 液相色谱

Abstract:

By not explicitly specifying the type of solvent strength model, the features of ladder-like gradient elution were studied based on the general retention time formula that was derived in our previous work. For the case where the solute is eluted at the slope of the ladder-like gradient, we derived the expression that connects the mobile phase composition (φR), at which the solute is eluted from the column, with the gradient slope (B). It was shown thatφR will increase with the increase of B in this case. For the case where the solute is eluted at the last isocratic segment of the ladder-like gradient, it was proven that the retention time (tR) will correlate linearly with the reciprocal of the gradient slope (1/B) when the initial and final mobile phase compositions are set to be constant. In experiments, by taking biphenyl as the sample, the values of retention time in isocratic and gradient elution were measured on a C18 column by using a mixture of methanol and water as the mobile phase. The experimental values were found to be well consistent with the theoretical values that were calculated from the expressions. These expressions will be helpful to understand the features of the ladder-like gradient in practice.

Key words: gradient elution, ladder-like gradient, liquid chromatography, retention factor

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