Abstract
Development of a chromatographic method in bioanalysis is a challenging and complex procedure with many pitfalls and often unexpected reversals that can require several months to accomplish. Even an experienced analytical team must contend many limitations mainly in connection with the strict requirements imposed on current clinical research. These restrictions typically persist throughout the whole development process, from clinical trial assignment, across optimization of extraction of biological materials and chromatographic separation, to validation and data interpretation. This paper describes questions and their possible answers raised during the pre-analytical phase such as use of modern sample preparation techniques in clinical methods, application of internal standards, as well as selection of stationary phases and detection techniques in the analytical phase. Validation problems and interpretation of results are demonstrated with three typical examples of characteristics to be considered, i.e. recovery, matrix effect, and limit of detection vs. lower limit of quantification.
Funding source: Charles University, Faculty of Pharmacy in Hradec Králové
Funding source: University Hospital in Hradec Králové
Funding source: Ministry of Health of the Czech Republic
Funding source: Ministry of Health of the Czech Republic
Funding source: Ministry of Health of the Czech Republic
Funding source: PERSONMED – Center for Development of Personalized Medicine in Age-Related Diseases
Funding source: STARSS project co-funded by ERDF
Acknowledgments
The authors gratefully acknowledge Filip Hátle for technical support. Thanks are also due for the financial support by Charles University, Faculty of Pharmacy in Hradec Králové (Project SVV 260 458), project MH CZ – DRO (University Hospital in Hradec Králové, 00179906), the Ministry of Health of the Czech Republic, grants numbers 18-03-00130, 17-28882A, and 17-29241A, PERSONMED – Center for Development of Personalized Medicine in Age-Related Diseases, Reg Nr. CZ.02.1.01/0.0/0.0/17_048/0007441 co-financed by the ERDF state budget of the Czech Republic. FS gratefully acknowledges the STARSS project (Reg. No. CZ.02.1.01/0.0/0.0/15_003/0000465) co-funded by ERDF.
-
Research funding: Thanks are due for the financial support by Charles University, Faculty of Pharmacy in Hradec Králové (Project SVV 260 458), project MH CZ – DRO (University Hospital in Hradec Králové, 00179906), the Ministry of Health of the Czech Republic, grant numbers 18-03-00130, 17-28882A, and 17-29241A, PERSONMED – Center for Development of Personalized Medicine in Age-Related Diseases, Reg Nr. CZ.02.1.01/0.0/0.0/17_048/0007441 co-financed by the ERDF state budget of the Czech Republic. FS gratefully acknowledges the STARSS project (Reg. No. CZ.02.1.01/0.0/0.0/15_003/0000465) co-funded by ERDF.
-
Author contributions: All authors have accepted responsibility for the entire content of this manuscript and approved its submission.
-
Competing interests: Authors state no conflict of interest.
References
1. World Health Organization. Clinical trials. Available from: https://www.who.int/topics/clinical_trials/en/ [Accessed 20 Sep 2019].Search in Google Scholar
2. Hammerling, JA. A review of medical errors in laboratory diagnostics and where we are today. Lab Med 2011;43:41–4. https://doi.org/10.1309/LM6ER9WJR1IHQAUY.Search in Google Scholar
3. Racek, J. Klinická biochemie, 2nd ed. Prague: Galén; 2006:23 p.Search in Google Scholar
4. Adaway, JE, Keevil, BG, Owen, LJ. Liquid chromatography tandem mass spectrometry in the clinical laboratory. Ann Clin Biochem 2014;52:18–38. https://doi.org/10.1177/0004563214557678.Search in Google Scholar PubMed
5. Hooshfar, S, Bastlett, MG. Hazards in chromatographic bioanalysis method development and applications. Biomed Chromatogr 2017;31:e3859. https://doi.org/10.1002/bmc.3859.Search in Google Scholar PubMed
6. Khamis, MM, Adamko, DJ, El-Aneed, A Strategies and challenges in method development and validation for the absolute quantification of endogenous biomarker metabolites using liquid chromatography-tandem mass spectrometry. Mass Spectrom Rev 2019;39:1–22. https://doi.org/10.1002/mas.21607.Search in Google Scholar PubMed
7. Patil, R, Bhaskar, R, Ola, M, Pingale, D, Chalikwar, S. Bioanalytical method development and method validation in human plasma by using LC MS/MS. Indo Am J Pharm 2019;06:5176–83.Search in Google Scholar
8. Kucerova, K, Kujovska Krcmova, L, Mikanova, Z, Matysova, L, Solich, P. Could urinary retinol be used as a new biomarker of kidney damage?. Trac-Trends Anal Chem 2017;95:57–61. https://doi.org/10.1016/j.trac.2017.07.025.Search in Google Scholar
9. Namera, A, Saito, T. Recent advances in unique sample preparation techniques for bioanalysis. Bioanalysis 2013;5:915–32. https://doi.org/10.4155/bio.13.52.Search in Google Scholar PubMed
10. Kabir, A, Locatelli, M, Ulusoy, HI. Recent trends in microextraction techniques employed in analytical and bioanalytical sample preparation. Separations 2017;4:1–15. https://doi.org/10.3390/separations4040036.Search in Google Scholar
11. Abdel-Rehim, M. Microextraction by packed sorbent in bioanalysis. Bioanalysis 2009;1:687–91. https://doi.org/10.4155/bio.09.61.Search in Google Scholar PubMed
12. Ahmadi, M, Elmongy, H, Madrakian, T, Abdel-Rehim, M. Nanomaterials as sorbents for sample preparation in bioanalysis: a review. Anal Chim Acta 2017;958:1–21. https://doi.org/10.1016/j.aca.2016.11.062.Search in Google Scholar PubMed
13. Zuloaga, O, Olivares, M, Navarro, P, Vallejo, A, Prieto, A. Dispersive liquid–liquid microextraction: trends in the analysis of biological samples. Bioanalysis 2015;7:2211–25. https://doi.org/10.4155/bio.15.141.Search in Google Scholar PubMed
14. Tang, YQ, Weng, N. Salting-out assisted liquid–liquid extraction for bioanalysis. Bioanalysis 2013;5:1583–98. https://doi.org/10.4155/bio.13.117.Search in Google Scholar PubMed
15. Ebrahomzadeh, H, Molaei, K, Asgharinezhad, AA, Shekari, N, Dehghani, Z. Molecularly imprinted nano particles combined with miniaturized homogenous liquid–liquid extraction for the selective extraction of loratadine in plasma and urine samples followed by high performance liquid chromatography-photo diode array detection. Anal Chim Acta 2013;767:155–62. https://doi.org/10.1016/j.aca.2013.01.013.Search in Google Scholar PubMed
16. Hamidi, S, Alipour-Ghorbani, N, Hamidi, A. Solid phase microextraction techniques in determination of biomarkers. Crit Rev Anal Chem 2018;48:239–51. https://doi.org/10.1080/10408347.2017.1396885.Search in Google Scholar PubMed
17. Filipou, O, Bitas, D, Samanidou, V. Green approaches in sample preparation of bioanalytical samples prior to chromatographic analysis. J Chromatogr B 2017;1043:44–62. https://doi.org/10.1016/j.jchromb.2016.08.040.Search in Google Scholar PubMed
18. Gjelstad, A, Andresen, AT, Dahlgren, A, Gundersen, TE, Pederson-Bjergaard, S. High-throughput liquid–liquid extraction in 96-well format: parallel artificial liquid membrane extraction. LC GC Eur 2017;30:10–7.Search in Google Scholar
19. Pan, J, Jiang, X, Chen, Y. Automatic supported liquid extraction (SLE) coupled with HILIC-MS/MS: an application to method development and validation of erlotinib in human plasma. Pharmaceutics 2010;2:105–18. https://doi.org/10.3390/pharmaceutics2020105.Search in Google Scholar PubMed PubMed Central
20. Bojko, B, Cudjoe, E, Pawliszyn, J, Wasowicz, M. Solid-phase microextraction. How far are we from clinical practice?. Trac-Trends Anal Chem 2011;30:1505–12. https://doi.org/10.1016/j.trac.2011.07.008.Search in Google Scholar
21. Srinivasan, B, Tung, S. Development and applications of portable biosensors. J Lab Autom 2015;20:365–89. https://doi.org/10.1177/2211068215581349.Search in Google Scholar PubMed
22. Filipiak, W, Bojko, B. SPME in clinical, pharmaceutical and biotechnological research – How far are we from daily practice?. Trac-Trends Anal Chem 2019;115:203–13. https://doi.org/10.1016/j.trac.2019.02.029.Search in Google Scholar
23. Kataoka, H, Saito, K. Recent advances in SPME techniques in biomedical analysis. J Pharmaceut Biomed 2011;54:926–50. https://doi.org/10.1016/j.jpba.2010.12.010.Search in Google Scholar PubMed
24. Roszkowska, A, Miekus, N, Baczek, T. Application of solid phase microextraction in current biomedical research. J Sep Sci 2019;42:285–302. https://doi.org/10.1002/jssc.201800785.Search in Google Scholar PubMed
25. Couchman, L. Turbulent flow chromatography in bioanalysis: a review. Biomed Chromatogr 2012;26:892–905. https://doi.org/10.1002/bmc.2769.Search in Google Scholar PubMed
26. Chromatography Today. Turbulent flow chromatography: an evolving solution for bioanalysis. Available from: https://www.chromatographytoday.com/article/bioanalytical/40/christophe_chassaing_sarah_robinson/turbulent_flow_chromatography_an_evolving_solution_for_bioanalysis/498 [Accessed: 14 Apr 2020].Search in Google Scholar
27. Michopoulos, F, Edge, AM, Theodoridis, G, Wilson, ID. Application of turbulent flow chromatography to the metabolomics analysis of human plasma: comparison with protein precipitation. J Sep Sci 2010;33:1472–79. https://doi.org/10.1002/jssc.200900789.Search in Google Scholar PubMed
28. Sahena, F, Zaidul, ISM, Jinap, S, Karim, AA, Abbas, KA, Norualini, NAN, et al. Application of supercritical CO2 in lipid extraction – a review. J Food Eng 2009;95:240–53. https://doi.org/10.1016/j.jfoodeng.2009.06.026.Search in Google Scholar
29. Rios, A, Zougagh, M, de Andres, F. Bioanalytical applications using supercritical fluid techniques. Bioanalysis 2010;2:9–25. https://doi.org/10.4155/bio.09.167.Search in Google Scholar PubMed
30. Adaway, JE, Keevil, BG, Owen, LJ. Liquid chromatography tandem mass spectrometry in the clinical laboratory. Ann Clin Biochem 2015;52:18–38. https://doi.org/10.1177/0004563214557678.Search in Google Scholar PubMed
31. Honour, JW. Development validation of a quantitative assay based on tandem mass spectrometry. Ann Clin Biochem 2011;48:97–111. https://doi.org/10.1258/acb.2010.010176.Search in Google Scholar PubMed
32. European Medicines Agency. Guideline on bioanalytical method validation. Available from: https://www.ema.europa.eu/ema/index.jsp?curl=pages/includes/document/documentdetail.jsp?webContentId=WC500109686%26mid=WC0b01ac058009a3dc [Accessed: 14 Apr 2020].Search in Google Scholar
33. U.S. Food and Drug Administration. Analytical procedures and methods validation for drugs and biologics. Available from: https://www.fda.gov/files/drugs/published/Analytical-Procedures-and-Methods-Validation-for-Drugs-and-Biologics.pdf [Accessed: 14 Apr 2020].Search in Google Scholar
34. Krcmova, L, Solichova, D, Plisek, J, Kasparova, M, Sobotka, L, Solich, P. Miniaturisation of solid phase extraction method for determination of retinol, alpha- and gamma-tocopherol in human serum using new technologies. Int J Environ Anal Chem 2010;90:106–14. https://doi.org/10.1080/03067310903267299.Search in Google Scholar
© 2020 Walter de Gruyter GmbH, Berlin/Boston
