[en] Supercritical Fluid Chromatography (SFC) has known a strong regain of interest for the last 10 years, especially in the field of pharmaceutical analysis. Besides the development and validation of the SFC method in one individual laboratory, it is also important to demonstrate its applicability and transferability to various laboratories around the world. Therefore, an inter-laboratory study was conducted and published for the first time in SFC, to assess method reproducibility, and evaluate whether this chromatographic technique could become a reference method for quality control (QC) laboratories. This study involved 19 participating laboratories from 4 continents and 9 different countries. It included 5 academic groups, 3 demonstration laboratories at analytical instrument companies, 10 pharmaceutical companies and 1 food company. In the initial analysis of the study results, consistencies within- and between-laboratories were deeply examined. In the subsequent analysis, the method reproducibility was estimated taking into account variances in replicates, between-days and between-laboratories. The results obtained were compared with the literature values for liquid chromatography (LC) in the context of impurities determination. Repeatability and reproducibility variances were found to be similar or better than those described for LC methods, and highlighted the adequacy of the SFC method for QC analyses. The results demonstrated the excellent and robust quantitative performance of SFC. Consequently, this complementary technique is recognized on equal merit to other chromatographic techniques.
Research center :
CIRM - Centre Interdisciplinaire de Recherche sur le Médicament - ULiège
Disciplines :
Pharmacy, pharmacology & toxicology Chemistry
Author, co-author :
Dispas, Amandine ; Université de Liège - ULiège > Département de pharmacie > Analyse des médicaments
Desfontaine, V., Guillarme, D., Francotte, E., Novakova, L., Supercritical fluid chromatography in pharmaceutical analysis. J. Pharm. Biomed. Anal. 113 (2015), 56–71.
Novakova, L., Plachka, K., Chapter 16 – pharmaceutical applications. Poole, C.F., (eds.) Supercritical Fluid Chromatography, 2017, Elsevier, Amsterdam, 461–494.
Dispas, A., Lebrun, P., Ziemons, E., Marini, R., Rozet, E., Hubert, P., Evaluation of the quantitative performances of supercritical fluid chromatography: from method development to validation. J. Chromatogr. A 1353 (2014), 78–88.
Dispas, A., Lebrun, P., Sacré, P.-Y., Hubert, Ph., Screening study of SFC critical method parameters for the determination of pharmaceutical compounds. J. Pharm. Biomed. Anal., 125, 2016 339-254.
Hicks, M., Regalado, E.L., Tan, F., Gong, X., Welch, C.J., Supercritical fluid chromatography for GMP analysis in support of pharmaceutical development and manufacturing activities. J. Pharm. Biomed. Anal. 117 (2016), 316–324.
Dispas, A., Desfontaine, V., Andri, B., Lebrun, P., Kotoni, D., Clarke, A., Guillarme, D., Hubert, Ph., Quantitative determination of salbutamol sulfate impurities using achiral supercritical fluid chromatography. J. Pharm. Biomed. Anal. 134 (2017), 170–180.
Dispas, A., Lebrun, P., Hubert, Ph., Validation of supercritical fluid chromatography methods. Poole, C., (eds.) Supercritical Fluid Chromatography, Handbook in Separation Science, 2017, Elsevier, 317–344.
International Organisation for Standardisation (ISO), Accuracy (trueness and Precision) of Measurements Methods and Results – Part 2: Basic Method for the Determination of Repeatability and Reproducibility of a Standard Measurement Method. 1994, International Standard ISO 5725-2(E).
Marini, R.D., Matthijs, N., Vander Heyden, Y., Smeyers-Berbeke, J., Dehouck, P., Hoogmartens, J., Silverstre, P., Ceccato, A., Goedert, Ph., Saevels, J., Herbots, C., Caliaro, G., Herraez-Hernandez, R., Verdu-Andres, J., Campins-Falco, P., Van de Wauw, W., De Beer, J., Boulanger, N., Chiap, P., Crommen, J., Hubert, Ph., Collaborative study of a liquid chromatographic method for the determination of R-timolol and other related substances in S-timolol maleate. Anal. Chim. Acta 546 (2005), 182–192.
Vander Heyden, Y., Saevels, J., Roets, E., Hoogmartens, J., Decolin, D., Quaglia, M.G., Van den Bossche, W., Leemans, R., Smeets, O., Van de Vaart, F., Mason, B., Taylor, G.C., Underberg, W., Bult, A., Chiap, P., Crommen, J., De Beer, J., Hansen, S.H., Massart, D.L., Inter-laboratory studies on two high-performance liquid chromatography assays for tylosin (tartrate). J. Chromatogr. A 830 (1999), 3–28.
Dehouck, P., Vander Heyden, Y., Smeyers-Verbeke, J., Massart, D.L., Marini, R., Chiap, P., Hubert, Ph., Crommen, J., Van de Wauw, W., De Beer, J., Cox, R., Mathiey, G., Reepmeyer, J.C., Voigt, B., Estevenon, O., Nicolas, A., Van Schepdael, A., Adams, E., Hoogmartens, J., Inter-laboratory study of a liquid chromatography method for erythromycin: determination of uncertainty. J. Chromatogr. A 1010 (2003), 63–74.
Dispas, A., Avohou, H.T., Lebrun, P., Hubert, Ph., Hubert, C., ‘Quality by Design’ approach for the analysis of impurities in pharmaceutical drug products and drug substances. TrAC 101 (2018), 24–33.
Vander Heyden, Y., Smeyers-Verbeke, J., Set-up and evaluation of inter-laboratory studies. J. Chromatogr. A 1158 (2007), 158–167.
Analytical Methods Committee, Uncertainty of measurement: implications of its use in analytical science. Analyst 120 (1995), 2303–2308.
PTS report, EDQM., 2017.
Horwitz, W., Kamps, L.R., Boyer, K.W., Quality assurance in the analysis of foods for trace constituents. J. Assoc. Off. Anal. Chem. 63 (1980), 1344–1354.