Interlaboratory study of a supercritical fluid chromatography method for the determination of pharmaceutical impurities: Evaluation of multi-systems reproducibility
[en] Modern supercritical fluid chromatography (SFC) is now a well-established technique, especially in the field of pharmaceutical analysis. We recently demonstrated the transferability and the reproducibility of a SFC-UV method for pharmaceutical impurities by means of an inter-laboratory study. However, as this study involved only one brand of SFC instrumentation (Waters®), the present study extends the purpose to multi-instrumentation evaluation. Specifically, three instrument types, namely Agilent®, Shimadzu®, and Waters®, were included through 21 laboratories (n = 7 for each instrument). First, method transfer was performed to assess the separation quality and to set up the specific instrument parameters of Agilent® and Shimadzu® instruments. Second, the inter-laboratory study was performed following a protocol defined by the sending lab. Analytical results were examined regarding consistencies within- and between-laboratories criteria. Afterwards, the method reproducibility was estimated taking into account variances in replicates, between-days and between-laboratories. Reproducibility variance was larger than that observed during the first study involving only one single type of instrumentation. Indeed, we clearly observed an ‘instrument type’ effect. Moreover, the reproducibility variance was larger when considering all instruments than each type separately which can be attributed to the variability induced by the instrument configuration. Nevertheless, repeatability and reproducibility variances were found to be similar than those described for LC methods; i.e. reproducibility as %RSD was around 15 %. These results highlighted the robustness and the power of modern analytical SFC technologies to deliver accurate results for pharmaceutical quality control analysis.
Research Center/Unit :
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
Clarke, Adrian
Grand-Guillaume Perrenoud, Alexandre
Losacco, Luca Gioacchino
Veuthey, Jean-Luc
Gros, Quentin
Molineau, Jérémy
Noireau, Angéline
West, Caroline
Salafia, Fabio
Zoccali, Mariosimone
Mondello, Luigi
Guillen, Amber
Wang, Jenny
Zhang, Kelly
Jochems, Philipp
Schad, Gesa
Nakajima, Kosuke
Horie, Shinnosuke
Joseph, Jan
Parr, Maria Kristina
Billemont, Pierre
Severino, Antoni
Schneider, Sonja
Naegele, Edgar
Kutscher, Daniel
Wikfors, Rick
Black, Regina
Ingvaldson, Lee
Oliviera Da Silva, Jimmy
Bennett, Raffeal
Regalado, Erik L.
Hoang, Thi Phuong Thuy
Touboul, David
Nikolova, Yana
Kamenova-Nacheva, Mariana
Dimitrov, Vladimir
Berger, Blair K.
Schug, Kevin A.
Kerviel-Guillon, Solène
Mauge, Fabien
Takahashi, Masatomo
Izumi, Yoshihiro
Bamba, Takkeshi
Rouvière, Florent
Heinisch, Sabine
Guillarme, Davy
Hubert, Philippe ; Université de Liège - ULiège > Département de pharmacie > Chimie analytique
Interlaboratory study of a supercritical fluid chromatography method for the determination of pharmaceutical impurities: Evaluation of multi-systems reproducibility
McClain, R., Chapter 1-milestones in supercritical fluid chromatography: a historical view of the modernization and development of supercritical fluid chromatography. Poole, C., (eds.) Supercritical Fluid Chromatography, Handbook in Separation Science, 2017, Elsevier, 1–21.
Tarafder, A., Metamorphosis of supercritical fluid chromatography to SFC: an overview. TrAC 81 (2016), 2–10, 10.1016/j.trac.2016.01.002.
Novakova, L., Plachka, K., Chapter 16 – pharmaceutical applications. Poole, C., (eds.) Supercritical Fluid Chromatography, Handbook in Separation Science, 2017, Elsevier, 461–494, 10.1016/B978-0-12-809207-1.00016-1.
Dispas, A., Lebrun, P., Hubert, Ph., Chapter 11 - validation of supercritical fluid chromatography methods. Poole, C., (eds.) Supercritical Fluid Chromatography, Handbook in Separation Science, 2017, Elsevier, 317–344, 10.1016/B978-0-12-809207-1.00011-2.
Pirrone, G.F., Mathew, R.M., Makarov, A.A., Bernardoni, F., Klapars, A., Hartman, R., Limanto, J., Regalado, Erik L., Supercritical fluid chromatography-photodiode array detection-electrospray ionization mass spectrometry as a framework for impurity fate mapping in the development and manufacture of drug substances. J. Chromatogr. B 1080 (2018), 42–49, 10.1016/j.jchromb.2018.02.006.
Hicks, M.B., 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, 10.1016/j.jpba.2015.09.014.
Khalikova, M.A., Lesellier, E., Chapuzet, E., Satinsky, D., West, W., Development and validation of ultra-high performance supercritical fluid chromatography method for quantitative determination of nine sunscreens in cosmetic samples. Anal. Chim. Acta 1034 (2018), 184–194, 10.1016/j.aca.2018.06.013.
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. 2019, International Standard ISO 5725-2 https://www.iso.org/fr/standard/69419.html.
Vander Heyden, Y., Smeyers-Verbeke, J., Set-up and evaluation of inter-laboratory studies. J. Chromatogr. A 1158 (2007), 158–167, 10.1016/j.chroma.2007.02.053.
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. Analytical Chimica Acta 546 (2005), 182–192, 10.1016/j.aca.2005.05.026.
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, 10.1016/j.jpba.2016.11.039.
Dispas, A., Marini, R., Desfontaine, V., Veuthey, J.-L., et al. First inter-laboratory study of a Supercritical Fluid Chromatography method for the determination of pharmaceutical impurities. J. Pharm. Biomed. Anal. 161 (2018), 414–424, 10.1016/j.jpba.2018.08.042.
Analytical Methods Committee, Uncertainty of measurement: implications of its use in analytical science. Analyst 120 (1995), 2303–2308, 10.1039/AN9952002303.
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, 10.1093/jaoac/63.6.1344.