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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 ELSD

  • Original Paper
  • Published:
Journal of the American Oil Chemists' Society

Abstract

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.

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Abbreviations

ANOVA:

Analysis of variance

ELSD:

Evaporative light scattering detector

FIA:

Flow injection analysis

HPLC:

High performance liquid chromatography

NLs:

Neutral lipids

PLs:

Polar lipids

RSM:

Response surface methodology

S/N ratio:

Signal to noise ratio

SPE:

Solid phase extraction

3D:

Three-dimensional

2D:

Two-dimensional

1st-D:

First-dimensional

2nd-D:

Second-dimensional

3rd-D:

Third-dimensional

References

  1. Cigic T, Blaz P, Vidrih R, Ulrih NP, Segatin N (2013) Correlation of basic oil quality indices and electrical properties of model vegetable oil systems. J Agric Food Chem 61:11355–11362

    Article  Google Scholar 

  2. Ruiz-Gutierrez V, Perez-Camino MC (2000) Update on solid-phase extraction for the analysis of lipid classes and related compounds. J Chromatogr A 885:321–341

    Article  CAS  Google Scholar 

  3. Karantonis HC, Antonopoulou S, Demopoulos CA (2002) Antithrombotic lipid minor constituents from vegetable oils comparison between olive oils and others. J Agric Food Chem 50:1150–1160

    Article  CAS  Google Scholar 

  4. Kaufman M, Wiesman Z (2007) Pomegranate oil analysis with emphasis on MALDI-TOF/MS triacylglycerol fingerprinting. J Agric Food Chem 55:10405–10413

    Article  CAS  Google Scholar 

  5. Nordback J, Lundberg E, Christie WW (1998) Separation of lipid classes from marine particulate material by HPLC on a polyvinyl alcohol-bonded stationary phase using dual-channel evaporative light-scattering detection. Mar Chem 60:165–175

    Article  CAS  Google Scholar 

  6. Lee WJ, Su NW, Lee MH, Lin JT (2013) Assessment of authenticity of sesame oil by modified Villavecchia test and HPLC-ELSD analysis of triacylglycerol profile. Food Res Int 53:195–202

    Article  Google Scholar 

  7. Compton D, Laszlo JA, Berhow MA (2006) Identification and quantification of feruloylated mono-, di-, and triacylglycerols from vegetable oils. J Am Oil Chem Soc 83:753–758

    Article  CAS  Google Scholar 

  8. Amaral JS, Cunha SC, Alves MR, Pereira JA, Seabra RM, Oliveira BPP (2004) Triacylglycerol composition of walnut (Juglans regia L.) cultivars: characterization by HPLC-ELSD and chemometrics. J Agric Food Chem 52:7964–7969

    Article  CAS  Google Scholar 

  9. Le TT, Miocinovic J, Nguyen TM, Rombaut R, Camp J, Dewettinck K (2011) Improved solvent extraction procedure and high-performance liquid chromatography evaporative light-scattering detector method for analysis of polar lipids from dairy materials. J Agric Food Chem 59:10407–10413

    Article  CAS  Google Scholar 

  10. Torres CF, Vazquez L, Senorans FJ, Reglero G (2005) Study of the analysis of alkoxyglycerols and other non-polar lipids by liquid chromatography coupled with evaporative light scattering detector. J Chromatogr A 1078:28–34

    Article  CAS  Google Scholar 

  11. Homan R, Anderson MK (1998) Rapid separation and quantitation of combined neutral and polar lipid classes by high-performance liquid chromatography and evaporative light-scattering mass detection. J Chromatogr B 708:21–26

    Article  CAS  Google Scholar 

  12. Silversand C, Haux C (1997) Improved high-performance liquid chromatographic method for the separation and quantification of lipid classes: application to fish lipids. J Chromatogr B 703:7–14

    Article  CAS  Google Scholar 

  13. Foglia TA, Jones KC (1997) Quantitation of neutral lipid mixtures using high performance liquid chromatography with light scattering detection. J Liq Chromatogr Relat Technol 20:1829–1838

    Article  CAS  Google Scholar 

  14. Bravi E, Perretti G, Montanari L (2006) Fatty acids by high-performance liquid chromatography and evaporative light-scattering detector. J Chromatogr A 1134:210–214

    Article  CAS  Google Scholar 

  15. Megoulas NC, Koupparis MA (2005) Twenty years of evaporative light scattering detection. Crit Rev Anal Chem 35:301–316

    Article  CAS  Google Scholar 

  16. Zhao J, Li SP, Yanga FQ, Li P, Wang YT (2006) Simultaneous determination of saponins and fatty acids in Ziziphus jujuba (Suanzaoren) by high performance liquid chromatography-evaporative light scattering detection and pressurized liquid extraction. J Chromatogr A 1108:188–194

    Article  CAS  Google Scholar 

  17. Klift EJC, Truyols GV, Claassen FW, Holthoon FL, Beek TA (2008) Comprehensive two-dimensional liquid chromatography with ultraviolet, evaporative light scattering and mass spectrometric detection of triacylglycerols in corn oil. J Chromatogr A 1178:43–55

    Article  Google Scholar 

  18. Mondello L, Beccaria M, Donato P, Cacciola F, Dugo G, Dugo P (2011) Comprehensive two-dimensional liquid chromatography with evaporative light scattering detection for the analysis of triacylglycerols in Borago officinalis. J Sep Sci 34:688–692

    Article  CAS  Google Scholar 

  19. Jandera P (2012) Comprehensive two-dimensional liquid chromatography—practical impacts of theoretical considerations. A review. Cent Eur J Chem 10(3):844–875

    Article  Google Scholar 

  20. Baeten V, Meurens M (1996) Detection of virgin olive oil adulteration by Fourier transform Raman spectroscopy. J Agric Food Chem 44:2225–2230

    Article  CAS  Google Scholar 

  21. Rodríguez-Alcalá LM, Fontecha J (2010) Major lipid classes separation of buttermilk, and cows, goats and ewes milk by high performance liquid chromatography with an evaporative light scattering detector focused on the phospholipid fraction. J Chromatogr A 1217:3063–3066

    Article  Google Scholar 

  22. Lundstedt T, Seifert E, Abramo L, Thelin B, Nyström Å, Pettersen J, Bergman R (1998) Experimental design and optimization. Chemometr Intell Lab Syst 42:3–40

    Article  CAS  Google Scholar 

  23. Brereton RG (1997) Multilevel multifactor designs for multivariate calibration. Analyst 122:1521–1529

    Article  CAS  Google Scholar 

  24. Memon FN, Ayyilidiz F, Kara H, Memon S, Kenar A, Topkafa M, Sherazi STH, Memon NA, Durmaz F, Tarhan I (2015) Application of central composite design for the optimization of on-line solid phase extraction of Cu2+ by calix[4]arene bonded silica resin. Chemometr Intell Lab Syst 146:158–168

    Article  CAS  Google Scholar 

  25. Navarrete-Bolanos JL, Jimnez-Islas H, Botello-Alvarez E, Rico-Martınez R (2002) Application of the response surface methodology for the design of a lixiviation process. Org Process Res Dev 6:841–846

    Article  CAS  Google Scholar 

  26. Van Nederkassel AM, Vijverman V, Massart DL, Vander Heyden Y (2005) Development of a Ginkgo biloba fingerprint chromatogram with UV and evaporative light scattering detection and optimization of the evaporative light scattering detector operating conditions. J Chromatogr A 1085:230–239

    Article  Google Scholar 

  27. Karatapanis AE, Fiamegos YC, Sakkas VA, Stalikas CD (2011) Effect of chromatographic parameters and detector settings on the response of HILIC–evaporative light-scattering detection system using experimental design approach and multicriteria optimization methodology. Talanta 83:1126–1133

    Article  CAS  Google Scholar 

  28. Coleman J, Wrzosek T, Roman R, Peterson J, McAllister P (2001) Setting system suitability criteria for delectability in high-performance liquid chromatography methods using signal-to-noise ratio statistical tolerance intervals. J Chromatogr A 917:23–27

    Article  CAS  Google Scholar 

  29. McLaren DG, Miller PL, Lassman ME, Castro-Perez JM, Hubbard BK, Roddy TP (2011) An ultraperformance liquid chromatography method for the normal-phase separation of lipids. Anal Biochem 414(2):266–272

    Article  CAS  Google Scholar 

Download references

Acknowledgments

The present study is a part of the Ph.D. thesis entitled “Integration of retarded and pre-concentrated SPE systems to FIA-HPLC systems for vegetable oil analysis and improvement of its applications”. The research was supported by TUBITAK with a 1001-The Support Program for Scientific and Technological Research Projects entitled “Developing a new SPE–FIA–HPLC hyphenated system for three-dimensional chromatographic analysis of vegetable oils with a single injection and their applications” with 112T373 Project number and Selcuk University Coordinators of Scientific Research with 12401045 and 11201063 Project numbers. The authors wish to thank the principal of TUBITAK and Selcuk University S.R.P. Coordination.

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Authors and Affiliations

  1. Department of Chemistry, Faculty of Science, University of Karamanoglu Mehmetbey, 70010, Karaman, Turkey

    Fatma Nur Arslan

  2. Department of Chemistry, Faculty of Science, University of Selcuk, 42075, Konya, Turkey

    Fatma Nur Arslan & Huseyin Kara

  3. Department of Biotechnology, Faculty of Science, University of Necmettin Erbakan, 42090, Konya, Turkey

    Huseyin Kara

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  1. Fatma Nur Arslan
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Correspondence to Fatma Nur Arslan.

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Arslan, F.N., Kara, H. 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 ELSD. J Am Oil Chem Soc 93, 11–26 (2016). https://doi.org/10.1007/s11746-015-2750-0

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  • DOI: https://doi.org/10.1007/s11746-015-2750-0

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