Fully Automated Three-Dimensional Column-Switching SPE–FIA–HPLC System for the Characterization of Lipids by a Single Injection: Part I. Instrumental Design and Chemometric Approach to Assess the Effect of Experimental Settings on the Response of ELS

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• 作者：Fatma Nur Arslan ; Huseyin Kara
• 关键词：Three ; dimensional (3D) separation ; Column ; switching ; ELSD ; Lipid ; Vegetable oil ; Chemometric
• 刊名：Journal of the American Oil Chemists' Society
• 出版年：2016
• 出版时间：January 2016
• 年：2016
• 卷：93
• 期：1
• 页码：11-26
• 全文大小：4,247 KB
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• 作者单位：Fatma Nur Arslan (1) (2)
  Huseyin Kara (2) (3)
  
  1. Department of Chemistry, Faculty of Science, University of Karamanoglu Mehmetbey, 70010, Karaman, Turkey
  2. Department of Chemistry, Faculty of Science, University of Selcuk, 42075, Konya, Turkey
  3. Department of Biotechnology, Faculty of Science, University of Necmettin Erbakan, 42090, Konya, Turkey
  
• 刊物类别：Chemistry and Materials Science
• 刊物主题：Chemistry
  Industrial Chemistry and Chemical Engineering
  Analytical Chemistry
  Chemistry
  Biotechnology
  Biomaterials
  Agriculture
  
• 出版者：Springer Berlin / Heidelberg
• ISSN：1558-9331

文摘

This article presents the first application of fully automated three-dimensional (3D) column-switching SPE–FIA–HPLC system for the characterization of lipids by a single injection. The whole system was designed and set up by modifying Agilent 1200 Series HPLC system in our laboratory. By using this system, a complete separation profile of the oil samples was achieved in a very short time period by using single injections. This approach was applied on vegetable oils which contains a large number of relatively high-class lipid components, such as TG, FFA, sterols, tocopherols, DG, ester and MG. In this part of the study, we focused on the optimization of evaporative light scattering detector (ELSD) by using an experimental design and RSM. Three experimental parameters were chosen as an independent variables which are the flow rate of mobile phase, nebulization temperature and evaporation temperature. A multivariate five level experimental design was used to establish a quadratic model as a functional relationship between the response values and independent variables. The optimal values of parameters were found to be a flow rate of 1.25 mL min−1, nebulization temperature of 80 °C, and evaporation temperature of 40 °C. Regression analysis with an R 2 values indicated as a satisfactory correlation between the experimental and predicted values. ANOVA test results were also illustrate that the models can be successfully used to predict the optimum parameters of ELSD. Thus, the proposed system is suitable for a large number of applications including research and development of new quality control and characterization methods for vegetable oils.