首页|液相色谱中线性溶剂强度模型的快速建立

液相色谱中线性溶剂强度模型的快速建立

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目的 通过一组单线性梯度洗脱实验获取线性溶剂强度模型的参数值，为色谱图的预测提供所必须的参数值。方法 首先，在实验中固定流动相组成的起始和结束值，通过改变梯度洗脱的时间，从而改变梯度的斜率(B)。测定溶质在这些梯度条件下的保留时间，计算其流出色谱柱时所对应的流动相组成(φR)。然后，将描述φR与B之间关系的数学公式对实验数据进行非线性拟合，从而获取线性溶剂强度模型的参数值。拟合基于Levenberg-Marquardt算法，通过Excel中的Visual Basic for Applications(VBA)语言编程实现。结果 计算机程序的可靠性通过实验进行验证。以12种芳环化合物为分离的对象，以C18柱为固定相，含1％乙酸的甲醇-水溶液为流动相，应用所编写的程序对单线性梯度洗脱实验数据进行处理，获取溶剂强度模型的参数值。然后，根据所得到的参数值预测多线性梯度洗脱条件下的色谱图，得到的理论色谱图与实验色谱图吻合。结论 所建立的方法可快速准确地获取线性溶剂强度模型的参数值，具有良好的实用价值。
Quick development of linear solvent strength model by in liquid chromatography
Objective By carrying out a set of single linear gradient experiments,the coefficients of linear solvent strength model(LSSM)were acquired for the prediction of liquid chromatogram.Methods Firstly,the initial and final values of mobile phase composition were fixed in experiments,and the time for gradient elution was varied so as to change the slope(B)of linear gradient.The retention times of analyte in the experiments were measured,and the values of mobile phase composition(φR)at which the solute is eluted from the column were calculated.Then,the formula accounting for the relationship between φR and B was fitted to experimental data,and the coefficients of LSSM were obtained by means of nonlinear fit which was implemented by means of a program written in house using Visual Basic for Applications(VBA)in Microsoft Excel.Results The reliability of the program was verified in experiments.Twelve aromatic compounds were chosen as analytes for HPLC separation.The stationary phase was a C18 column,and the mobile phase was a mixture of methanol and water containing 1％(v/v)acetic acid.The computer program was applied to analyze the experimental data obtained from single linear gradient elution,and the coefficients of LSSM were consequently acquired.Then,the chromatogram under multilinear gradient elution was predicted based on the LSSM coefficients acquired.It is found that the experimental and predicted chromatograms are well consistent.Conclusion The method developed in this work can be used to obtain the coefficients of LSSM quickly and accurately and thus has a good value for practical use.

Liquid chromatographyGradient elutionLinear solvent strength modelVisual Basic for ApplicationsNonlinear fittingLevenberg-Marquardt algorithm

阚育洵、郝卫强、徐瑾、蒋磊

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常州工程职业技术学院检验检测认证学院,常州 213164

液相色谱 梯度洗脱 线性溶剂强度模型 VBA 非线性拟合 Levenberg-Marquardt算法

江苏省自然科学基金江苏省"333工程"科研资助项目江苏省高等学校基础科学(自然科学)研究项目江苏省高校优秀科技创新团队项目

BK20201164BRA202031022KJD350001苏教科[2023]3号

2024

10.11876/mimt202402006

现代仪器与医疗
中国科学器材公司

现代仪器与医疗

影响因子：1.47
ISSN：2095-5200
年,卷(期)：2024.30(2)
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