[en] In the last years, supercritical fluid chromatography has largely been acknowledged as a singular and performing technique in the field of separation sciences. Recent studies highlighted the interest of SFC for the quality control of pharmaceuticals, especially in the case of the determination of the active pharmaceutical ingredient (API).Nevertheless, quality control requires also the determination of impurities. The objectives of the present work were to i) demonstrate the interest of SFC as a reference technique for the determination of impurities in salbutamol sulfate API and ii) to propose an alternative to a reference HPLC method from the European Pharmacopeia (EP) involving ionpairing
reagent. Firstly, a screening was carried out to select the most adequate and selective stationary phase. Secondly, in the context of robust optimization strategy, the method was developed using design space methodology. The separation of salbutamol sulfate and related impurities was achieved in 7 minutes, which is seven times faster than the LC-UV method proposed by European Pharmacopeia (total run time of 50 minutes). Finally, full validation using accuracy profile approach was successfully achieved for the determination of impurities B, D, F and G in salbutamol sulfate raw material. The validated dosing range covered 50 to 150 % of the targeted concentration (corresponding to 0.3 % concentration level), LODs close to 0.5 μg/mL were estimated. The SFC method proposed in this study could be presented as a suitable fast alternative to EP LC method for the quantitative determination of salbutamol impurities.
Disciplines :
Chemistry Pharmacy, pharmacology & toxicology
Author, co-author :
Dispas, Amandine ; Université de Liège > Département de pharmacie > Chimie analytique
Desfontaine, Vincent
Andri, Bertyl ; Université de Liège > Département de pharmacie > Chimie analytique
Lebrun, Pierre ; Université de Liège > Département de pharmacie > Chimie analytique
Kotoni, Dorina
Clarke, Adrian
Guillarme, Davy
Hubert, Philippe ; Université de Liège > Département de pharmacie > Chimie analytique
Language :
English
Title :
Quantitative determination of salbutamol sulfate impurities using achiral supercritical fluid chromatography
[1] Gourmel, C., Perrenoud, A.G.-G., Waller, L., Reginato, E., Verne, J., Dulery, B., Veuthey, J.-L., Rudaz, S., Schappler, J., Guillarme, D., Evaluation and comparison of various separation techniques for the analysis of closely-related compounds of pharmaceutical interest. J. Chromatogr. A 1281 (2013), 172–177.
[2] Perrenoud, A.G.-G., Farrell, W.P., Aurigemma, C.M., Aurigemma, N.C., Feteke, S., Guillarme, D., Evaluation of stationary phases packed with superficially porous particles for the analysis of pharmaceutical compounds using supercritical fluid chromatography. J. Chromatogr. A 1360 (2014), 257–287.
[3] Galea, C., Mangelings, D., Vander Heyden, Y., Method development for impurity profiling in SFC: the selection of a dissimilar set of stationary phases. J. Pharm. Biomed. Anal. 111 (2015), 333–343.
[4] 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), 339–354.
[5] Dispas, A., Lebrun, P., Ziemons, E., Marini, R., Rozet, E., Hubert, Ph., Evaluation of the quantitative performances of supercritical fluid chromatography: from method development to validation. J. Chromatogr. A 1353 (2014), 78–88.
[6] Marley, A., Connolly, D., Determination of (R)-timolol in (S)-timolol maleate active pharmaceutical ingredient: validation of a new supercritical fluid chromatography method with an established normal phase liquid chromatography method. J. Chromatogr. A, 1325, 2014, 220.
[7] 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.
[8] Li, W., Wang, J., Yan, Z.-Y., Development of a sensitive and rapid method for rifampicin impurity analysis using supercritical fluid chromatography. J. Pharm. Biomed. Anal. 114 (2015), 341–347.
[9] Alexander, A.J., Zhang, L., Hooker, T.F., Tomasella, F.P., Comparison of supercritical fluid chromatography and reverse liquid chromatography for the impurity profiling of the antiretroviral drugs lamivudine/BMS-986001/efavirens in a combination tablet. J. Pharm. Biomed. Anal. 78-79 (2013), 243–251.
[10] Salbutamol sulfate, monograph 01/2008:0687, European pharmacopeia 6.0.
[11] The International Conference of Harmonization of Technical Requirements for Registration of Pharmaceuticals for Human Use; Q8 R2 Pharmaceutical Development, htt://www/ich.org/fileadmin/Public_Web_Site/ICH_Products/Guidelines/Quality/Q8_RI/Step4/Q8_R2_Guidelines.pdf.
[12] Nethercote, P., Ermer, J., Quality by design for analytical methods: implications for method validation and transfer. Pharm. Technol. 36 (2012), 52–55.
[13] Rozet, E., Lebrun, P., Debrus, B., Boulanger, B., Hubert, P., Design spaces for analytical methods. TrAC 42 (2013), 157–167.
[14] Borman, P., Nethercote, P., Chatfield, M., Thompson, D., Truman, K., The applicability of quality by design to analytical method. Pharm. Technol. 31 (2007), 142–152.
[15] Peterson, J.J., What your ICH Q8 Design Space needs: a multivariate predictive distribution. Pharm. Manuf. Mag., 2010.
[16] Lebrun, P., Boulanger, B., Debrus, B., Lambert, Ph., Hubert, Ph., A Bayesian design space for analytical methods based on multivariate models and predictions. J. Biopharm. Stat. 23 (2013), 1330–1351.
[17] Dejaegher, B., Vander Heyden, Y., Ruggedness and robustness testing. J. Chromatogr. A. 1158 (2007), 138–157.
[18] Dispas, A., Lebrun, P., Sassiat, P., Ziémons, E., Thiébaut, D., Vial, J., Hubert, Ph., Innovative green supercritical fluid chromatography development for the determination of polar compounds. J. Chromatogr. A 1256 (2012), 253–260.
[19] U.S. Pharmacopeial Convention, new chapter 1224, 1225, 1226, USP panel expert.
[20] Hubert, Ph., Nguyen-Huu, J.J., Boulanger, B., Chapuzet, E., Chiap, P., Cohen, N., Compagnon, P.A., Dewé, W., Feinberg, M., Lallier, M., Laurentie, M., Mercier, N., Muzard, G., Nivet, C., Valat, L., Harmonization of strategies for the validation of quantitative analytical procedures–a SFSTP proposal–part I. J. Pharm. Biomed. Anal. 36 (2004), 579–586.
[21] Hubert, Ph., Nguyen-Huu, J.J., Boulanger, B., Chapuzet, E., Chiap, P., Cohen, N., Compagnon, P.A., Dewé, W., Feinberg, M., Lallier, M., Laurentie, M., Mercier, N., Muzard, G., Nivet, C., Valat, L., Rozet, E., Harmonization of strategies for the validation of quantitative analytical procedures–a SFSTP proposal–part II. J. Pharm. Biomed. Anal. 45 (2007), 70–81.
[22] Hubert, Ph., Nguyen-Huu, J.-J., Boulanger, B., Chapuzet, E., Cohen, N., Compagnon, P.-A., Dewé, W., Feinberg, M., Laurentie, M., Mercier, N., Muzard, G., Valat, L., Rozet, E., Harmonization of strategies for the validation of quantitative analytical procedures–a SFSTP proposal–part III. J. Pharm. Biomed. Anal. 45 (2007), 82–96.
[23] Hubert, Ph., Nguyen-Huu, J.-J., Boulanger, B., Chapuzet, E., Cohen, N., Compagnon, P.-A., Dewé, W., Feinberg, M., Laurentie, M., Mercier, N., Muzard, G., Valat, L., Rozet, E., Harmonization of strategies for the validation of quantitative analytical procedures–a SFSTP proposal–Part IV. J. Pharm. Biomed. Anal. 48 (2008), 760–771.
[24] Perrenoud, A.G.-G., Boccard, J., Veuthey, J.-L., Guillarme, D., Analysis of basic compounds by supercritical fluid chromatography: attempts to improve peak shape and maintain mass spectrometry compatibility. J. Chromatogr. A 1262 (2012), 205–213.
[25] The R project https://www.r-project.org.
[26] West, C., Lesellier, E., A unified classification of stationary phases for packed column supercritical fluid chromatography. J. Chromatogr. A 1191 (2008), 21–39.
[27] West, C., Lemasson, E., Bertin, S., Hennig, Ph., Lesellier, E., An improved classification of stationary phases for ultra-high performance supercritical fluid chromatography. J. Chromatogr. A 1440 (2016), 212–228.
[28] West, C., Khalikova, M.A., Lesellier, E., Héberger, K., Sum of ranking differences to rank stationary phases used in packed column supercritical fluid chromatography. J. Chromatogr. A 1409 (2015), 241–250.
[29] Desfontaine, V., Veuthey, J.-L., Guillarme, D., Evaluation of innovative stationary phase ligand chemistries and analytical conditions for the analysis of basic drugs by supercritical fluid chromatography. J. Chromatogr. A 1438 (2016), 244–253.
[30] Lesselier, E., West, C., The many faces of packed column supercritical fluid chromatography. J. Chromatogr. A 1382 (2015), 2–46.
[31] The international Conference of Harmonization of Technical Requirements for Registration of Pharmaceuticals for Human Use; Q2 R1 Validation of analytical procedures: text and methodology, http://www.ich.org/fileadmin/Public_Web_Site/ICH_Products/Guidelines/Quality/Q2_R1/Step4/Q2_R1__Guideline.pdf.
[32] USP 38, Chapter 1225–Validation of Compendial Procedures.
[33] Miller, J.C., Miller, J.N., Statistics for Analytical Chemistry. 3rd ed., 1993, Ellis Horwood, New York.