title: Retrospective data analysis and proposal of a practical acceptance criterion for inter-laboratory cross-validation of bioanalytical methods using liquid chromatography/tandem mass spectrometry.
abstract: The purpose of this study is to conduct a retrospective data analysis for inter-laboratory cross-validation studies to set a reasonable and practical acceptance criterion based on a number of cross-validation results. From the results of cross-validation studies for 16 compounds and their metabolites, analytical bias and variation were evaluated. The accuracy of cross-validation samples was compared with that of quality control (QC) samples with statistical comparison of the analytical variation. An acceptance criterion was derived with a confidential interval approach. As the results, while a larger bias was observed for the cross-validation samples, the bias was not fully caused by analytical variation or bias attributable to the analytical methods. The direction of the deviation between the cross-validation samples and QC samples was random and not concentration-dependent, suggesting that inter-laboratory variability such as preparation errors could be a source of bias. A derived acceptance criterion corresponds to one prescribed in the Guideline on bioanalytical method validation from the Ministry of Health, Labour and Welfare in Japan and is a little wider than one in the European Medical Agency. In conclusion, thorough retrospective data analysis revealed potential causes of larger analytical bias in inter-laboratory cross-validation studies. A derived acceptance criterion would be practical and reasonable for the inter-laboratory cross-validation study.
authors.affiliation: Drug Metabolism and Pharmacokinetics Research Laboratories, Pharmaceutical Research Division, Takeda Pharmaceutical Company Limited, 26-1, Muraoka-higashi 2-chome, Fujisawa, Kanagawa, 251-8555, Japan, tomoki.yoneyama@takeda.com.
authors.forename: Tomoki
authors.initials: T
authors.lastname: Yoneyama
authors.forename: Takashi
authors.initials: T
authors.lastname: Kudo
authors.forename: Fumihiro
authors.initials: F
authors.lastname: Jinno
authors.forename: Eric R
authors.initials: ER
authors.lastname: Schmidt
authors.forename: Takahiro
authors.initials: T
authors.lastname: Kondo
mesh_terms: D002138:Calibration; D002853:Chromatography, Liquid / Q000295:instrumentation / Q000379:methods*; D019963:Clinical Chemistry Tests / Q000592:standards*; D006801:Humans; D007753:Laboratories / Q000592:standards*; D059021:Laboratory Proficiency Testing / Q000379:methods / Q000592:standards*; D004364:Pharmaceutical Preparations / Q000097:blood / Q000378:metabolism / Q000652:urine; D017410:Practice Guidelines as Topic; D012015:Reference Standards; D012189:Retrospective Studies; D053719:Tandem Mass Spectrometry / Q000295:instrumentation / Q000379:methods*; D054928:Validation Studies as Topic
chemical_list: D004364:Pharmaceutical Preparations