Skip to main content
Log in

Retention mechanism assessment and method development for the analysis of iohexol and its related compounds in hydrophilic interaction liquid chromatography

  • Research Paper
  • Published:
Analytical and Bioanalytical Chemistry Aims and scope Submit manuscript

Abstract

Hydrophilic interaction liquid chromatography (HILIC) has emerged in recent years as a valuable alternative to reversed-phase liquid chromatography in the analysis of polar compounds. Research in HILIC is divided into two directions: the assessment of the retention mechanism and retention behavior, and the development of HILIC methods. In this work, four polar neutral analytes (iohexol and its related compounds A, B, and C) were analyzed on two silica and two diol columns in HILIC mode with the aim to investigate thoroughly the retention mechanisms and retention behavior of polar neutral compounds on these four columns. The adsorption and partition contribution to the overall HILIC retention mechanism was investigated by fitting the retention data to linear (adsorption and partition) and nonlinear (mixed-retention and quadratic) theoretical models. On the other hand, the establishment of empirical second-order polynomial retention models on the basis of D-optimal design made possible the estimation of the simultaneous influence of several mobile-phase-related factors. Furthermore, these models were also used as the basis for the application of indirect modeling of the selectivity factor and a grid point search approach in order to achieve the optimal separation of analytes. After the optimization goals had been set, the grids were searched and the optimal conditions were identified. Finally, the optimized method was subjected to validation.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Fig. 1
Fig. 2
Fig. 3
Fig. 4
Fig. 5

Similar content being viewed by others

References

  1. Hemstrom P, Irgum K (2006) Hydrophilic interaction chromatography. J Sep Sci 29:1784–1821

    Article  Google Scholar 

  2. Jandera P (2011) Stationary and mobile phases in hydrophilic interaction chromatography: a review. Anal Chim Acta 692:1–25

    Article  CAS  Google Scholar 

  3. Buszewski B, Noga S (2012) Hydrophilic interaction chromatography (HILIC) – a powerful separation technique. Anal Bioanal Chem 402:231–247

    Article  CAS  Google Scholar 

  4. United States Pharmacopeial Convention (2012) United States pharmacopeia 35. United States Pharmacopeial Convention, Rockville

    Google Scholar 

  5. Edelson J, Palace G, Park G (1983) Pharmacokinetics of iohexol, a new nonionic radiocontrast agent, in humans. J Chromatogr B 274:428–433

    Article  CAS  Google Scholar 

  6. Krutzen E, Back SE, Nilsson-Ehle I, Nilsson-Ehle P (1984) Plasma clearance of a new contrast agent, iohexol: a method for the assessment of glomerular filtration rate. J Lab Clin Med 104:955–961

    CAS  Google Scholar 

  7. Brändström E, Grzegorczyk A, Jacobsson L, Friberg P, Lindahl A, Aurell M (1998) GFR measurement with iohexol and 51Cr-EDTA. A comparison of the two favoured GFR markers in Europe. Nephrol Dial Transplant 13:1176–1182

    Article  Google Scholar 

  8. Shihabi ZK, Thompson EN, Constantinescu MS (1993) Iohexol determination by direct injection of serum on the HPLC column. J Liq Chromatogr 16:1289–1296

    Article  CAS  Google Scholar 

  9. Farthing D, Sica DA, Fakhry I, Larus T, Ghosh S, Farthing C, Vranian M, Gehr T (2005) Simple HPLC-UV method for determination of iohexol, iothalamate, p-aminohippuric acid and n-acetyl-p-aminohippuric acid in human plasma and urine with ERPF, GFR and ERPF/GFR ratio determination using colorimetric analysis. J Chromatogr B 826:267–272

    Article  CAS  Google Scholar 

  10. Soman RS, Zahir H, Akhlaghi F (2005) Development and validation of an HPLC-UV method for determination of iohexol in human plasma. J Chromatogr B 816:339–343

    Article  CAS  Google Scholar 

  11. Cavalier E, Rozet E, Dubois N, Charlier C, Hubert P, Chapelle JP, Krzesinski JM, Delanaye P (2008) Performance of iohexol determination in serum and urine by HPLC: validation, risk and uncertainty assessment. Clin Chim Acta 396:80–85

    Article  CAS  Google Scholar 

  12. Castagnet S, Blasco H, Vourc'h P, Benz-De-Bretagne I, Veyrat-Durebex C, Barbet C, Alnajjar A, Andres CR (2012) Routine determination of GFR in renal transplant recipients by HPLC quantification of plasma iohexol concentrations and comparison with estimated GFR. J Clin Lab Anal 26:376–383

    Article  CAS  Google Scholar 

  13. Lee SY, Chun MR, Kim DJ, Kim JW (2006) Determination of iohexol clearance by high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). J Chromatogr B 839:124–129

    Article  CAS  Google Scholar 

  14. Annesley TM, Clayton LT (2009) Ultraperformance liquid chromatography-tandem mass spectrometry assay for iohexol in human serum. Clin Chem 55:1196–1202

    Article  CAS  Google Scholar 

  15. Denis MC, Venne K, Lesiège D, Francoeur M, Groleau S, Guay M, Cusson J, Furtos A (2008) Development and evaluation of a liquid chromatography-mass spectrometry assay and its application for the assessment of renal function. J Chromatogr A 1189:410–416

    Article  CAS  Google Scholar 

  16. De Baere S, Smets P, Finch N, Heiene R, De Backer P, Daminet S, Croubels S (2012) Quantitative determination of exo- and endo-iohexol in canine and feline samples using high performance liquid chromatography with ultraviolet detection. J Pharm Biomed Anal 61:50–56

    Article  Google Scholar 

  17. Liu J, Cai M, Tan L, Ji HY, Shi JP, Wang Y (2010) Simultaneous determination of two related compounds in iohexol and its injection by LC-MS/MS. Chin Pharm J 45:468–471

    CAS  Google Scholar 

  18. Poole CF (2003) The essence of chromatography. Elsevier, Amsterdam

    Google Scholar 

  19. Snyder LR, Dolan JW, Gant JR (1979) Gradient elution in high-performance liquid chromatography. I. Theoretical basis for reversed-phase systems. J Chromatogr A 165:3–30

    Article  CAS  Google Scholar 

  20. Snyder LR (1974) Role of the solvent in liquid-solid chromatography - a review. Anal Chem 46:1384–1393

    Article  CAS  Google Scholar 

  21. Jin G, Guo Z, Zhang F, Xue X, Jin Y, Liang X (2008) Study on the retention equation in hydrophilic interaction liquid chromatography. Talanta 76:522–527

    Article  CAS  Google Scholar 

  22. Rozet E, Lebrun P, Debrus B, Boulanger B, Hubert P (2013) Design spaces for analytical methods. Trends Anal Chem 42:157–167

    Article  CAS  Google Scholar 

  23. De Aguiar PF, Bourguignon B, Khots MS, Massart DL, Phan-Than-Luu R (1995) D-optimal designs. Intel Lab 30:199–210

    Article  CAS  Google Scholar 

  24. Kumar A, Heaton JC, McCalley DV (2013) Practical investigation of the factors that affect the selectivity in hydrophilic interaction chromatography. J Chromatogr A 1276:33–46

    Article  CAS  Google Scholar 

  25. Alpert A (1990) Hydrophilic-interaction chromatography for the separation of peptides, nucleic acids and other polar compounds. J Chromatogr 449:177–196

    Article  Google Scholar 

  26. Karatapanis AE, Fiamegos YC, Stalikas CD (2011) A revisit to the retention mechanism of hydrophilic interaction liquid chromatography using model organic compounds. J Chromatogr A 1218:2871–2879

    Article  CAS  Google Scholar 

  27. McCalley DV (2010) Study of the selectivity, retention mechanisms and performance of alternative silica-based stationary phases for separation of ionised solutes in hydrophilic interaction chromatography. J Chromatogr A 1217:3408–3417

    Article  CAS  Google Scholar 

  28. Dinh NP, Jonsson T, Irgum K (2011) Probing the interaction mode in hydrophilic interaction chromatography. J Chromatogr A 1218:5880–5891

    Article  CAS  Google Scholar 

  29. Dewé W, Marini RD, Chiap P, Hubert P, Crommen J, Boulanger B (2004) Development of response models for optimising HPLC methods. Chemometer Intell Lab 74:263–268

    Article  Google Scholar 

  30. Lebrun P, Govaerts B, Debrus B, Ceccato A, Caliaro G, Hubert P, Boulanger B (2008) Development of a new predictive modelling technique to find with confidence equivalence zone and design space of chromatographic analytical methods. Chemometer Intell Lab 91:4–16

    Article  CAS  Google Scholar 

  31. Crowther JB (2001) In: Ahuja S, Scypinski S (eds) Handbook of modern pharmaceutical analysis, 2nd edn. New York, Academic

    Google Scholar 

Download references

Acknowledgments

The authors thank the Ministry of Education, Science, and Technological Development of the Republic of Serbia for supporting these investigations in project 172052.

Author information

Authors and Affiliations

Authors

Corresponding author

Correspondence to Biljana Jančić-Stojanović.

Rights and permissions

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Jovanović, M., Rakić, T., Jančić-Stojanović, B. et al. Retention mechanism assessment and method development for the analysis of iohexol and its related compounds in hydrophilic interaction liquid chromatography. Anal Bioanal Chem 406, 4217–4232 (2014). https://doi.org/10.1007/s00216-014-7808-6

Download citation

  • Received:

  • Revised:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s00216-014-7808-6

Keywords

Navigation