色谱

色谱 ›› 2015, Vol. 33 ›› Issue (12): 1274-1286.DOI: 10.3724/SP.J.1123.2015.06037

• 研究论文 • 上一篇    下一篇

丁基柱保留机理的化学计量学研究:pH和pKa的影响和关系(英文)

KOUSKOURA Maria G, MITANI Constantina V, MARKOPOULOU Catherine K   

  1. Laboratory of Pharmaceutical Analysis, Department of Pharmaceutical Technology, School of Pharmacy, Faculty of Health Sciences, Aristotle University of Thessaloniki, 54124 Thessaloniki, Greece
  • 收稿日期:2015-06-23 出版日期:2015-12-08 发布日期:2012-06-21
  • 通讯作者: MARKOPOULOU Catherine K

Chemometric study of the retention mechanism on butyl column: effect and relation of pH and pKa

KOUSKOURA Maria G, MITANI Constantina V, MARKOPOULOU Catherine K   

  1. Laboratory of Pharmaceutical Analysis, Department of Pharmaceutical Technology, School of Pharmacy, Faculty of Health Sciences, Aristotle University of Thessaloniki, 54124 Thessaloniki, Greece
  • Received:2015-06-23 Online:2015-12-08 Published:2012-06-21

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摘要：

Reversed phase chromatographic separations are optimized for analytes containing ionizable groups by adjustment of pH of mobile phases. As it seems the pKa values of compounds affect their retention because of the variety in their solvation. However, it is of stressful need to predict their behavior taking into account also a series of other parameters. This work focuses on the development of ten different models, using partial least squares regression, which will identify and quantify the impact of several factors in the chromatographic behavior of 104 analytes. The combined effect of their numerous characteristics is obvious since along with pH (at 2.3 and 6.2), factors such as lipophilicity, molecular volume, polar surface area and the presence of specific moieties in their structures are not diminished. On the contrary, they work increasing or counterbalancing several effects on the retention time. The models compiled can be applied to predict with reliability (R2>0.865 and Q2>0.777) the behavior of unknown drugs.

关键词: butyl column, ionization percentage, pKa, partial least squares regression

Abstract:

Reversed phase chromatographic separations are optimized for analytes containing ionizable groups by adjustment of pH of mobile phases. As it seems the pKa values of compounds affect their retention because of the variety in their solvation. However, it is of stressful need to predict their behavior taking into account also a series of other parameters. This work focuses on the development of ten different models, using partial least squares regression, which will identify and quantify the impact of several factors in the chromatographic behavior of 104 analytes. The combined effect of their numerous characteristics is obvious since along with pH (at 2.3 and 6.2), factors such as lipophilicity, molecular volume, polar surface area and the presence of specific moieties in their structures are not diminished. On the contrary, they work increasing or counterbalancing several effects on the retention time. The models compiled can be applied to predict with reliability (R2>0.865 and Q2>0.777) the behavior of unknown drugs.

Key words: butyl column, ionization percentage, pKa, partial least squares regression

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