Desharnais, Brigitte ORCID: https://orcid.org/0000-0001-7373-656X, Camirand-Lemyre, Félix ORCID: https://orcid.org/0000-0003-3277-2729, Mireault, Pascal and Skinner, Cameron D. (2017) Procedure for the selection and validation of a calibration model: II —Theoretical basis. Journal of Analytical Toxicology, 41 (4). pp. 269-276. ISSN 0146-4760
Preview |
Text (Post-print of the main article: final draft post-refereeing) (application/pdf)
292kBCalibration II - Theory.pdf - Accepted Version Available under License Spectrum Terms of Access. |
Spreadsheet (Supplemental Data 1) (application/vnd.openxmlformats-officedocument.spreadsheetml.sheet)
20kBSupplemental Data 1.xlsx - Supplemental Material Available under License Spectrum Terms of Access. | |
Preview |
Text (Supplemental Data 2) (application/pdf)
48kBSupplemental Data 2.pdf - Supplemental Material Available under License Spectrum Terms of Access. |
Official URL: https://doi.org/10.1093/jat/bkx002
Abstract
In the first part of this paper (I — Description and application), an automated, stepwise and analyst independent process for the selection and validation of calibration models was put forward and applied to two model analytes. This second part presents the mathematical reasoning and experimental work underlying the selection of the different components of this procedure. Different replicate analysis designs (intra/inter-day and intra/interextraction) were tested and their impact on test results was evaluated. For most methods, the use of intra-day/intra-extraction measurement replicates is recommended due to its decreased variability. This process should be repeated three times during the validation process in order to assess the time stability of the underlying model. Strategies for identification of heteroscedasticity and their potential weaknesses were examined and a unilateral F-test using the lower limit of quantification and upper limit of quantification replicates was chosen. Three different options for model selection were examined and tested: ANOVA lack-of-fit (LOF), partial F-test and significance of the second-order term. Examination of mathematical assumptions for each test and LC-MS/MS experimental results lead to selection of the partial F-test as being the most suitable. The advantages and drawbacks of ANOVA-LOF, examination of the standardized residuals graph and residuals normality testing (Kolmogorov-Smirnov or Cramer-Von Mises) for validation of the calibration model were examined with the last option proving the best in light of its robustness and accuracy. Choosing the correct calibration model improves QC accuracy, and simulations have shown that this automated scheme has a much better performance than a more traditional method of fitting with increasingly complex models until QC accuracies pass below a threshold.
Divisions: | Concordia University > Faculty of Arts and Science > Chemistry and Biochemistry |
---|---|
Item Type: | Article |
Refereed: | Yes |
Authors: | Desharnais, Brigitte and Camirand-Lemyre, Félix and Mireault, Pascal and Skinner, Cameron D. |
Journal or Publication: | Journal of Analytical Toxicology |
Date: | 1 February 2017 |
Projects: |
|
Funders: |
|
Digital Object Identifier (DOI): | 10.1093/jat/bkx002 |
Keywords: | Calibration, calibration model, quadratic, linear, weighted calibration, validation, heteroscedastic, standardized residuals, ANOVA lack-of-fit, significance of the second order term, forcing through the origin |
ID Code: | 984861 |
Deposited By: | BRIGITTE DESHARNAIS |
Deposited On: | 10 Jan 2019 15:05 |
Last Modified: | 10 Jan 2019 15:05 |
Related URLs: |
References:
[1] Peters, Frank T and Drummer, Olaf H and Musshoff, Frank, Validation of new methods, Forensic Science International 165 (2007) 216–224.[2] Scientific Working Group for Forensic Toxicology, Scientific Working Group for Forensic Toxicology (SWGTOX) Standard Practices for Method Validation in Forensic Toxicology, Journal of Analytical Toxicology 37 (2013) 452–474.
[3] Shah, Vinod P and Midha, Kamal K and Findlay, John WA and Hill, Howard M and Hulse, James D and McGilveray, Iain J and McKay, Gordon and Miller, Krys J and Patnaik, Rabindra N and Powell, Mark L and others, Bioanalytical method validation - a revisit with a decade of progress, Pharmaceutical Research 17 (2000) 1551–1557.
[4] F. T. Peters, Method validation using LC-MS, in: A. Polettini (Ed.), Applications of LC-MS in Toxicology, Pharmaceutical Press, London, United Kingdom, 2006, pp. 71–96.
[5] Hartmann, C and Smeyers-Verbeke, J and Massart, DL and McDowall, RD, Validation of bioanalytical chromatographic methods, Journal of Pharmaceutical and Biomedical Analysis 17 (1998) 193–218.
[6] Penninckx, W and Hartmann, C and Massart, DL and Smeyers-Verbeke, J, Validation of the calibration procedure in atomic absorption spectrometric methods, Journal of Analytical Atomic Spectrometry 11 (1996) 237–246.
[7] H. Gu, G. Liu, J. Wang, A.-F. Aubry, M. E. Arnold, Selecting the correct weighting factors for linear and quadratic calibration curves with least-squares regression algorithm in bioanalytical LCMS/ MS assays and impacts of using incorrect weighting factors on curve stability, data quality, and assay performance, Analytical Chemistry 86 (2014) 8959–8966.
[8] Burrows, John and Watson, Kenneth, Linearity of chromatographic systems in drug analysis part I: theory of nonlinearity and quantification of curvature, Bioanalysis 7 (2015) 1731–1743.
[9] Pagliano, Enea and Mester, Zolt´an and Meija, Juris, Calibration graphs in isotope dilution mass spectrometry, Analytica Chimica Acta 896 (2015) 63–67.
[10] Hubert, Ph and Chiap, Patrice and Crommen, Jacques and Boulanger, Bruno and Chapuzet, E and Mercier, N and Bervoas-Martin, S and Chevalier, P and Grandjean, D and Lagorce, Ph and others, The SFSTP guide on the validation of chromatographic methods for drug bioanalysis: from the Washington Conference to the laboratory, Analytica Chimica Acta 391 (1999) 135–148.
[11] Moore, Christine and Rana, Sumandeep and Coulter, Cynthia, Determination of meperidine, tramadol and oxycodone in human oral fluid using solid phase extraction and gas chromatography–mass spectrometry, Journal of Chromatography B 850 (2007) 370–375.
[12] Cociglio, M and Peyriere, H and Hillaire-Buys, D and Alric, R, Application of a standardized coextractive cleanup procedure to routine high-performance liquid chromatography assays of teicoplanin and ganciclovir in plasma, Journal of Chromatography B: Biomedical Sciences and Applications 705 (1998) 79–85.
[13] Gupta, Anubha and Jansson, Britt and Chatelain, Pierre and Massingham, Roy and Hammarlund-Udenaes, Margareta, Quantitative determination of cetirizine enantiomers in guinea pig plasma, brain tissue and microdialysis samples using liquid chromatography/tandem mass spectrometry, Rapid Communications in Mass Spectrometry 19 (2005) 1749–1757.
[14] Peters, Frank T. and Maurer, Hans H., Bioanalytical method validation and its implications for forensic and clinical toxicology — A review, in: De Bi`evre, Paul and G¨unzler, Helmut (Ed.), Validation in Chemical Measurement, Springer, Berlin, Germany, 2005, pp. 1–9.
[15] D.L. Massart, B.G.M. Vandeginste, L.M.C Buydens, S. De Jong, P.J. Lewi, J. Smeyers-Verbeke, Straight Line Regression and Calibration, in: Handbook of Chemometrics and Qualimetrics: Part A, volume 20A of Data Handling in Science and Technology, Elsevier, Amsterdam, Netherlands, 1997, pp. 171–230.
[16] Rozet, Eric and Ceccato, Attilio and Hubert, C´edric and Ziemons, Eric and Oprean, Radu and Rudaz, Serge and Boulanger, Bruno and Hubert, Philippe, Analysis of recent pharmaceutical regulatory documents on analytical method validation, Journal of Chromatography A 1158 (2007) 111–125.
[17] D.L. Massart, B.G.M. Vandeginste, L.M.C Buydens, S. De Jong, P.J. Lewi, J. Smeyers-Verbeke, Some important hypothesis tests, in: Handbook of Chemometrics and Qualimetrics: Part A, volume 20A of Data Handling in Science and Technology, Elsevier, Amsterdam, Netherlands, 1997, pp. 93–120.
[18] D.L. Massart, B.G.M. Vandeginste, L.M.C Buydens, S. De Jong, P.J. Lewi, J. Smeyers-Verbeke, Multiple and Polynomial Regression, in: Handbook of Chemometrics and Qualimetrics: Part A, volume 20A of Data Handling in Science and Technology, Elsevier, Amsterdam, Netherlands, 1997, pp. 263–303.
[19] Karnes, H Thomas and Shiu, Gerald and Shah, Vinod P, Validation of bioanalytical methods, Pharmaceutical Research 8 (1991) 421–426.
[20] Cook, R. D. and Weisberg, S., Diagnostic methods using residuals, in: Residuals and influence in regression, Chapman and Hall, New York, United States of America, 1982, pp. 10–100.
[21] Gonz´alez, A Gustavo and Herrador, M ´Angeles, A practical guide to analytical method validation, including measurement uncertainty and accuracy profiles, Trends in Analytical Chemistry 26 (2007) 227–238.
[22] Darling, Donald A, The kolmogorov-smirnov, cramer-von mises tests, The Annals of Mathematical Statistics 28 (1957) 823–838.
[23] Miller, James and Miller, Jane C, Statistics of repeated measurements, in: Statistics and chemometrics for analytical chemistry, Pearson Education, Harlow, England, 6 edition, 2010, pp. –37–73.
[24] van der Vaart, Aad W. and Wellner, Jon A., The Bootstrap, in: Weak Convergence and Empirical Processes: With Applications to Statistics, Springer, New York, United States of America, 1996, pp. 345–359.
[25] Desharnais, Brigitte and Camirand-Lemyre, F´elix and Mireault, Pascal and Skinner, Cameron D, Determination of confidence intervals in non-normal data: application of the bootstrap to cocaine concentration in femoral blood, Journal of Analytical Toxicology 39 (2015) 113–117.
[26] Wellner, Jon A. Wellner and van der Vaart, Aad W., Empirical processes indexed by estimated functions, in: Asymptotics: Particles, Processes and Inverse Problems, volume 55 of Lecture Notes- Monograph Series, Institute of Mathematical Statistics, 2007, pp. 234–252.
[27] Zhao, Yue and Liu, Guowen and Shen, Jim X and Aubry, Anne-Francoise, Reasons for calibration standard curve slope variation in LC–MS assays and how to address it, Bioanalysis 6 (2014) 1439–1443.
[28] Hubert, Ph and Nguyen-Huu, J-J and Boulanger, Bruno and Chapuzet, E and Cohen, N and Compagnon, P-A and Dew´e, Walth`ere and Feinberg, M and Laurentie, Michel and Mercier, N and others, Harmonization of strategies for the validation of quantitative analytical procedures: A SFSTP proposal–Part III, Journal of Pharmaceutical and Biomedical Analysis 45 (2007) 82–96.
[29] Ingle, James D. and Crouch, Stanley R., Signal-to-Noise Ratio Considerations, in: Spectrochemical Analysis, Prentice Hall, Englewood Cliffs, United States of America, 1988, pp. 135–163.
[30] Lanckmans, Katrien and Clinckers, Ralph and Van Eeckhaut, Ann and Sarre, Sophie and Smolders, Ilse and Michotte, Yvette, Use of microbore LC–MS/MS for the quantification of oxcarbazepine and its active metabolite in rat brain microdialysis samples, Journal of Chromatography B 831 (2006) 205–212.
[31] Apostolou, Constantinos and Dotsikas, Yannis and Kousoulos, Constantinos and Loukas, Yannis L, Development and validation of an improved high-throughput method for the determination of anastrozole in human plasma by LC–MS/MS and atmospheric pressure chemical ionization, Journal of Pharmaceutical and Biomedical Analysis 48 (2008) 853–859.
[32] Nilsson, Lars B and Eklund, G¨oran, Direct quantification in bioanalytical LC–MS/MS using internal calibration via analyte/stable isotope ratio, Journal of Pharmaceutical and Biomedical Analysis 43 (2007) 1094–1099.
Repository Staff Only: item control page