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八种头孢菌素在不同固定相上的色谱亲脂性评估。

Assessment of the chromatographic lipophilicity of eight cephalosporins on different stationary phases.

作者信息

Dąbrowska Monika, Starek Małgorzata, Komsta Łukasz, Szafrański Przemysław, Stasiewicz-Urban Anna, Opoka Włodzimierz

机构信息

Department of Inorganic and Analytical Chemistry, Faculty of Pharmacy, Jagiellonian University Medical College, 9 Medyczna St, 30-688 Krakow, Poland.

Department of Inorganic and Analytical Chemistry, Faculty of Pharmacy, Jagiellonian University Medical College, 9 Medyczna St, 30-688 Krakow, Poland.

出版信息

Eur J Pharm Sci. 2017 Apr 1;101:115-124. doi: 10.1016/j.ejps.2017.01.034. Epub 2017 Jan 28.

Abstract

The retention behaviors were investigated for a series of eight cephalosporins in thin-layer chromatography (TLC) using stationary phases of RP-2, RP-8, RP-18, NH, DIOL, and CN chemically bonded silica gel. Additionally, various binary mobile phases (water/methanol and water/acetone) were used in different volume proportions. The retention behavior of the analyzed molecules was defined by R constant. In addition, reversed phase high performance liquid chromatography (RP-HPLC) was performed in lipophilicity studies by using immobilized artificial membrane (IAM) stationary phase. Obtained chromatographic data (R and logk') were correlated with the lipophilicity, expressed as values of the log calculated (logP) and experimental (logP) partition coefficient. Principal component analysis (PCA) was applied in order to obtain an overview of similarity or dissimilarity among the analyzed compounds. Hierarchical cluster analysis (HCA) was performed to compare the separation characteristics of the applied stationary phases. This study was undertaken to identify the best chromatographic system and chromatographic data processing method to enable the prediction of logP values. A comprehensive chromatographic investigation into the retention of the analyzed cephalosporins revealed a similar behavior on RP-18, RP-8 and CN stationary phases. The weak correlations obtained between experimental and certain computed lipophilicity indices revealed that R and PC1/RM are relevant lipophilicity parameters and the RP-8, CN and RP-18 plates are appropriate stationary phases for lipophilicity investigation, whereas computational approaches still cannot fully replace experimentation.

摘要

使用RP - 2、RP - 8、RP - 18、NH、二醇和CN化学键合硅胶作为固定相,在薄层色谱(TLC)中研究了一系列8种头孢菌素的保留行为。此外,还使用了不同体积比例的各种二元流动相(水/甲醇和水/丙酮)。分析分子的保留行为由R值定义。此外,在亲脂性研究中,通过使用固定化人工膜(IAM)固定相进行反相高效液相色谱(RP - HPLC)。获得的色谱数据(R和logk')与亲脂性相关,亲脂性用计算得到的logP值和实验得到的logP分配系数表示。应用主成分分析(PCA)以获得被分析化合物之间相似性或差异性的概述。进行层次聚类分析(HCA)以比较所应用固定相的分离特性。进行这项研究是为了确定最佳的色谱系统和色谱数据处理方法,以便能够预测logP值。对所分析头孢菌素保留情况的全面色谱研究表明,在RP - 18、RP - 8和CN固定相上行为相似。实验值与某些计算得到的亲脂性指数之间的弱相关性表明,R和PC1/RM是相关的亲脂性参数,RP - 8、CN和RP - 18板是用于亲脂性研究的合适固定相,而计算方法仍不能完全取代实验。

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