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采用 Box-Behnken 设计评估亲水相互作用色谱法中β-内酰胺类抗生素的保留情况。

Assessment of β-lactams retention in hydrophilic interaction chromatography applying Box-Behnken design.

机构信息

University of Belgrade, Department of Drug Analysis, Faculty of Pharmacy, Belgrade, Serbia.

出版信息

J Sep Sci. 2012 Jun;35(12):1424-31. doi: 10.1002/jssc.201200099.

DOI:10.1002/jssc.201200099
PMID:22740252
Abstract

In this paper, the retention prediction models for mixture of β-lactam antibiotics analyzed by hydrophilic interaction chromatography (HILIC) are presented. The aim of the study was to investigate the retention behavior of some organic acids and amphoteric compounds including cephalosporins (cefotaxime, cefalexin, cefaclor, cefuroxime, and cefuroxime axetil) and penicillins (ampicillin and amoxicillin). Retention of substances with acidic functional group in HILIC is considered to be interesting since the majority of publications in literature are related to basic compounds. In the beginning of the study, classical silica columns were chosen for the retention analysis. Then, preliminary study was done and factors with the most significant influence on the retention factors were selected. These factors with the impact on the retention factors were investigated employing Box-Behnken design as a tool. On the basis of the obtained results the mathematical models were created and tested using ANOVA test and finally verified. This approach enables the presentation of chromatographic retention in many ways (three-dimensional (3-D) graphs and simple two-dimensional graphical presentations). All of these gave the possibility to predict the chromatographic retention under different conditions. Furthermore, regarding the structure of the analyzed compounds, the potential retention mechanisms in HILIC were suggested.

摘要

本文介绍了用亲水作用色谱(HILIC)分析β-内酰胺抗生素混合物的保留预测模型。本研究的目的是研究一些有机酸和两性化合物(包括头孢菌素类[头孢噻肟、头孢氨苄、头孢克洛、头孢呋辛和头孢呋辛酯]和青霉素类[氨苄西林和阿莫西林])的保留行为。由于文献中的大多数出版物都与碱性化合物有关,因此具有酸性官能团的物质在 HILIC 中的保留是很有趣的。在研究开始时,选择了经典的硅胶柱进行保留分析。然后,进行了初步研究,选择了对保留因子有最显著影响的因素。采用 Box-Behnken 设计作为工具研究了这些对保留因子有影响的因素。根据获得的结果,创建了数学模型,并通过方差分析(ANOVA)进行了测试,最后进行了验证。这种方法可以用多种方式(三维(3-D)图和简单的二维图形表示)来表示色谱保留。所有这些都使得可以在不同条件下预测色谱保留。此外,根据所分析化合物的结构,提出了在 HILIC 中潜在的保留机制。

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