Chapter 11 - Validation of Supercritical Fluid Chromatography Methods

[en] Method validation is the process of proving that an analytical method is acceptable for its intended purpose. The present chapter defines the validation criteria described in regulatory documents. Despite the abundance of guidelines, the conclusion about method validity remains confused. In this context, the state-of-the-art validation methodology named total error approach is briefly explained as the methodology that should be followed for all method validations. Finally, a review of literature presents quantitative development and validation of supercritical fluid chromatography (SFC) methods considering a wide range of applications and analytical fields.

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 > Département de pharmacie > Chimie analytique

Lebrun, Pierre ; Université de Liège > Département de pharmacie > Chimie analytique

Hubert, Philippe ; Université de Liège > Département de pharmacie > Chimie analytique

Language :

English

Title :

Chapter 11 - Validation of Supercritical Fluid Chromatography Methods

Publication date :

2017

Main work title :

Supercritical Fluid Chromatography - Handbook in Separation Science

Editor :

Poole, Colin

Publisher :

Elsevier

Peer reviewed :

Peer reviewed

Available on ORBi :

since 20 March 2017

Statistics

Number of views

149 (17 by ULiège)

Number of downloads

3 (3 by ULiège)

More statistics

Scopus citations^®

Scopus citations^®
without self-citations

OpenCitations

OpenAlex citations

Bibliography

USP 38, Chapter 1225-Validation of Compendial Procedures.
Analytical procedures and methods validation for drugs and biologics-guidance for industry. U.S. Department of Health and Human Services, Food and Drug Administration; July 2015, <>. http://www.fda.gov/downloads/drugs/guidancecomplianceregulatoryinformation/guidances/ucm386366.pdf.
Eudralex Volume 4, Part 1-Chapter 6: Quality control, October 2014, <>. http://ec.europa.eu/health/files/eudralex/vol-4/2014-11_vol4_chapter_6.pdf.
International conference on harmonization of technical requirements for registration of pharmaceuticals for human use. Validation of analytical procedures: text and methodology Q2(R1), 2005; <>. http://www.ich.org/fileadmin/Public_Web_Site/ICH_Products/Guidelines/Quality/Q2_R1/Step4/Q2_R1__Guideline.pdf.
SO 17025, General requirements for the competence of calibration and testing laboratories, 2005.
Rozet E., Ceccato A., Hubert C., Ziemons E., Oprean R., Rudaz S., et al. Analysis of recent pharmaceutical regulatory documents on analytical method validation. J Chromatogr A 2007, 1158:111-125.
Bouabidi A., Rozet E., Fillet M., Ziemons E., Chapuzet E., Mertens B., et al. J Chromatogr A 2010, 1217:3180-3192.
Vial J., Jardy A. Experimental comparison of the different approaches to estimate LOD and LOQ of an HPLC method. Anal Chem 1999, 71:2672-2677.
International conference on harmonization of technical requirements for registration of pharmaceuticals for human use, Pharmaceutical development Q8(R1), 2009; <>. http://www.ich.org/fileadmin/Public_Web_Site/ICH_Products/Guidelines/Quality/Q8_R1/Step4/Q8_R2_Guideline.pdf.
Hubert P., Nguyen-Huu J.J., Boulanger B., Chapuzet E., Chiap P., Cohen N., et al. Harmonization of strategies for the validation of quantitative analytical procedures-a SFSTP proposal - part I. J Pharm Biomed Anal 2004, 36:579-586.
Hubert P., Nguyen-Huu J.J., Boulanger B., Chapuzet E., Chiap P., Cohen N., et al. Harmonization of strategies for the validation of quantitative analytical procedures-a SFSTP proposal - part II. J Pharm Biomed Anal 2007, 45:70-81.
Hubert P., Nguyen-Huu J.-J., Boulanger B., Chapuzet E., Cohen N., Compagnon P.-A., et al. Harmonization of strategies for the validation of quantitative analytical procedures-a SFSTP proposal - part III. J Pharm Biomed Anal 2007, 45:82-96.
Hubert P., Nguyen-Huu J.-J., Boulanger B., Chapuzet E., Cohen N., Compagnon P.-A., et al. Harmonization of strategies for the validation of quantitative analytical procedures-a SFSTP proposal - part IV. J Pharm Biomed Anal 2008, 48:760-771.
International conference on harmonization of technical requirements for registration of pharmaceuticals for human use, Quality Risk management Q9, 2005; <>. http://www.ich.org/fileadmin/Public_Web_Site/ICH_Products/Guidelines/Quality/Q9/Step4/Q9_Guideline.pdf.
Boulanger B, Devanaryan V, Dewé W, Smith W. Statistical considerations in analytical method validation, in Pharmaceutical Statistics, SAS Press, p. 69-94.
USP 1210, Statistical tools for procedure validation, chapter in process revision.
Mee R.W. β-Expectation and β-content tolerance limits for balanced one-way ANOVA pandom model. Technometrics 1984, 26:251-254.
International conference on harmonization of technical requirements for registration of pharmaceuticals for human use. Pharmaceutical development Q8(R2), 2009.
Nethercote P., Ermer J. Quality by design for analytical methods: implications for method validation and transfer. Pharm Tech 2012, 36:52-55.
Rozet E., Lebrun P., Debrus B., Boulanger B., Hubert P. Design spaces for analytical methods. Trends Anal Chem 2013, 42:157-167.
Borman P., Truman K., Thompson D., Nethercote P., Chatfield M. The application of Quality by Design to analytical methods. Pharm Tech 2007, 31:142-152.
Peterson J.J. What your ICH Q8 Design Space needs: a multivariate predictive distribution. Pharm Manuf 2010, Date of publication: 25 JUNE 2010.
Lebrun P., Boulanger B., Debrus B., Lambert P., Hubert P. A Bayesian design space for analytical methods based on multivariate models and predictions. J Biopharm Stat 2013, 23:1330-1351.
Dejaegher B., Heyden Y.V. Ruggedness and robustness testing. J Chromatogr A 2007, 1158:138-157.
Dispas A., Lebrun P., Sassiat P., Ziemons E., Thiébaut D., Vial J., et al. Innovative green supercritical fluid chromatography development for the determination of polar compounds. J Chromatogr A 2012, 1256:253-260.
Dispas A., Lebrun P., Andri B., Rozet E., Hubert P. Robust method optimization strategy, a useful tool for method transfer: the case of SFC. J Pharm Biomed Anal 2014, 88:519-524.
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 2014, 1353:78-88.
Hubert C, Houari S, Rozet E, Lebrun P, Hubert P. Towards a full integration of optimization and validation phases: an analytical-quality-by-design approach. J Chromatogr A, Vol. 1395, p. 22 May 2015, 88-98.
Rozet E., Dewé W., Ziemons E., Bouklouze A., Boulanger B., Hubert P. Methodologies for the transfer of analytical methods: a review. J Chromatogr B 2009, 877:2214-2223.
Rozet E., Mertens B., Dewe W., Ceccato A., Govaerts B., Boulanger B., et al. The transfer of LC-UV method for the determination of fenofibrate and fenofibric acid in Lidoses: use total error as decision criterion. J Pharm Biomed Anal 2006, 42:64-70.
Lee J.W., Nishiumi S., Yoshida M., Fukusaki E., Bamba T. Simultaneous profiling of polar lipids by supercritical fluid chromatography/tandem mass spectrometry with methylation. J Chromatogr A 2013, 1279:98-107.
Jumaah F., Larsson S., Essén S., Cunico L.P., Holm C., Turner C., et al. A rapid method for the separation of vitamin D and its metabolites by ultra-high performance supercritical fluid chromatography-mass spectrometry. J Chromatogr A 2016, 2440:191-200.
Coe R.A., Rathe J.O., Lee J.W. Supercritical fluid chromatography-tandem mass spectrometry for fast bioanalysis of R/S-warfarin in human plasma. J Pharm Biomed Anal 2006, 42:573-580.
Hsieh Y., Li F., Duncan C.J.G. Supercritical fluid chromatography and high-performance liquid chromatography/tandem mass spectrometric methods for the determination of cytarabine in mouse plasma. Anal Chem 2007, 79:3856-3861.
Liu X.-G., Qi L.-W., Fan Z.-Y., Dong X., Guo R.-Z., Lou F.-C., et al. Accurate analysis of ginkgolides and their hydrolyzed metabolites by analytical supercritical fluid chromatography hybrid tandem mass spectrometry. J Chromatogr A 2015, 1388:251-258.
Liu M., Zhao L., Yang D., Ma J., Wang X., Zhang T. Preclinical pharmacokinetic evaluation of a new formulation of bifendate solid dispersion using a supercritical fluid chromatography-tandem mass spectrometry method. J Pharm Biomed Anal 2014, 100:387-392.
Yang Z, Xu X, Sun L, Zhao X, Wang H, Fawcett JP, et al. Development and validation of an enantioselective SFC-MS/MS method for simultaneous separation and quantification of oxcarbazepine and its chiral metabolites in beagle dog plasma. J Chromatogr B; Vol. 1020, p. 1 May 2016, 36-42, <>. doi:10.1016/j.jchromb.2016.03.013.
Novakova L., Rentsch M., Perrenoud A.G.-G., Nicoli R., Saugy M., Veuthey J.-L., et al. Ultra high performance supercritical fluid chromatography coupled with tandem mass spectrometry for screening of doping agents. II: analysis of biological samples. Anal Chim Acta 2015, 853:647-659.
Novakova L., Desfontaine V., Ponzetto F., Nicoli R., Saugy M., Veuthey J.-L., et al. Fast and sensitive supercritical fluid chromatography-tandem mass spectrometry multi-class screening method for the determination of doping agents in urine. Anal Chim Acta 2016, 915:102-110.
Lesellier E., Mith D., Dubrulle I. Method developments approaches in supercritical fluid chromatography applied to the analysis of cosmetics. J Chromatogr A 2015, 1423:158-168.
Khater S., West C. Development and validation of a supercritical fluid chromatography method for the direct determination of enantiomeric purity of provitamin B5 in cosmetic formulations with mass spectrometric detection. J Pharm Biomed Anal 2015, 102:321-325.
Toyo'oka T., Kikura-Hanajiri R. A reliable method for the separation and detection of synthetic cannabinoids by supercritical fluid chromatography with mass spectrometry, and its application to plant products. Chem Pharm Bull 2015, 63:762-769.
Chen Z., Dong F., Li S., Zheng Z., Xu Y., Xu J., et al. Response surface methodology for the enantionseparation of dinotefuran and its chiral metabolite in bee products and environmental samples by supercritical fluid chromatography/tandem mass spectrometry. J Chromatogr A 2015, 1410:181-189.
Abramsson V., Rodriguez-Meizoso I., Turner C. Determination of carotenoids in microalgae using supercritical fluid extraction and chromatography. J Chromatogr A 2012, 1250:63-68.
Khalikova M.A., Satinsky D., Solich P., Novakova L. Development and validation of ultra-high performance supercritical fluid chromatography method for determination of illegal dyes and comparison to ultra-high performance liquid chromatography method. Anal Chim Acta 2015, 874:84-96.
Wang Z., Zhang H., Liu O., Donovan B. Development of an orthogonal method for mometasone furoate impurity analysis using supercritical fluid chromatography. J Chromatogr A 2011, 1218:2311-2319.
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 2014, 1325:213-220.
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 2016, 117:316-324.
Plachka K., Chrenkova L., Dousa M., Novakova L. Development, validation and comparison of UHPSFC and UHPLC methods for the determinataion of agomelatine and its impurities. J Pharm Biomed Anal 2016, 125:376-384.
DePhilippo T., Chen R. Separation and quantitative determination of hydrocortisone in Cortizone 10 Plus crème by supercritical fluid chromatography (SFC). LCGC Europe 2008, 21:37-38.
Méjean M., Vollmer M., Brunelle A., Touboul D. Quantification of retinoid compounds by supercritical fluid chromatography coupled to ultraviolet diode array detection. Chromatographia 2013, 76:1097-1105.
Desai P.P., Patel N.R., Sherikar O.D., Mehta P.J. Development and validation of packed column supercritical fluid chromatographic technique for quantification of chloroxazone, paracetamol and aceclofenac in their individual and combined dosage forms. J Chromatogr Sci 2012, 50:769-774.
Mukherjee P.S. Validation of direct assay of an aqueous formulation of a drug compound AZY by chiral supercritical fluid chromatography (SFC). J Pharm Biomed Anal 2007, 43:464-470.
Prajapati P., Agrawal Y.K. SFC-MS/MS for identification and simultaneous estimation of the isoniazid and pyrazinamide in its dosage form. J supercrit fluids 2014, 95:597-602.
Baudelet D., Schifano-Faux N., Ghinet A., Dezitter X., Barbotin F., Gautret P., et al. Enantioseparation of pyroglutamide derivatives on polysaccharide based chiral stationary phases by ultra-high performance chromatography and supercritical fluid chromatography: a comparative study. J Chromatogr A 2014, 1363:257-269.
Lecoeur M., Decaudin B., Guillotin Y., Sautou V., Vaccher C. Comparison of high-performance liquid chromatography and supercritical fluid chromatography using evaporative light scattering detection for the determination of platicizers in medical devices. J Chromatogr A 2015, 1417:104-115.
Dispas A., Lebrun P., Sacré P.-Y., Hubert P. Screening study of SFC critical method parameters for the determination of pharmaceutical compounds. J Pharm Biomed Anal 2016, 125:339-354.
European Medicines Agency. Guideline on bioanalytical method validation; 2011.
AFNOR NF. V03-110 (2010), Protocole de caractérisation en vue de la validation d'une méthode d'analyse quantitative par construction du profil d'exactitude.