AAPS J. 2014 Nov;16(6):1143-8. doi: 10.1208/s12248-014-9650-3. Epub 2014 Sep 5.
Method transfer, partial validation, and cross validation: recommendations for best practices and harmonization from the global bioanalysis consortium harmonization team.
This paper presents the recommendations of the Global Bioanalytical Consortium Harmonization Team on method transfer, partial validation, and cross validation. These aspects of bioanalytical method validation, while important, have received little detailed attention in recent years. The team has attempted to define, separate, and describe these related activities, and present practical guidance in how to apply these techniques.
Biomed Chromatogr. 2014 Sep;28(9):1212-8. doi: 10.1002/bmc.3148. Epub 2014 Apr 22.
An improved LC-MS/MS method for quantitation of indapamide in whole blood: application for a bioequivalence study.
An improved LC-MS/MS method for the quantitation of indapamide in human whole blood was developed and validated. Indapamide-d3 was used as internal standard (IS) and liquid-liquid extraction was employed for sample preparation. LC separation was performed on Synergi Polar RP-column (50 × 4.6 mm i.d.; 4 µm) and mobile phase composed of methanol and 5 mm aqueous ammonium acetate containing 1 mm formic acid (60:40), at flow rate of 1 mL/min. The run time was 3.0 min and the injection volume was 20 μL. Mass spectrometric detection was performed using electrospray ion source in negative ionization mode, using the transitions m/z 364.0 → m/z 188.9 and m/z 367.0 → m/z 188.9 for indapamide and IS, respectively. Calibration curve was constructed over the range 0.25-50 ng/mL. The method was precise and accurate, and provided recovery rates >80% for indapamide and IS. The method was applied to determine blood concentrations of indapamide in a bioequivalence study with two sustained release tablet formulations. The 90% confidence interval for the geometric mean ratios for maximum concentration was 95.78% and for the area under the concentration-time curve it was 97.91%. The tested indapamide tablets (Eurofarma Laboratórios S.A.) were bioequivalent to Natrilix®, according to the rate and extent of absorption.
Copyright © 2014 John Wiley & Sons, Ltd.
AAPS J. 2014 Mar;16(2):352-6. doi: 10.1208/s12248-014-9566-y. Epub 2014 Feb 6.
Recommendations and best practices for reference standards and reagents used in bioanalytical method validation.
The continued globalization of pharmaceutics has increased the demand for companies to know and understand the regulations that exist across the globe. One hurdle facing pharmaceutical and biotechnology companies developing new drug candidates is interpreting the current regulatory guidance documents and industry publications associated with bioanalytical method validation (BMV) from each of the different agencies throughout the world. The objective of this commentary is to provide our opinions on the best practices for reference standards and key reagents, such as metabolites and internal standards used in the support of regulated bioanalysis based on a review of current regulatory guidance documents and industry white papers for BMV.
Biomed. Chromatogr. 2012 Nov 16;26(11):1399-407. Epub 2012 Feb 16.
In the present study a simple, fast, sensitive and robust method to quantify mirtazapine in human plasma using quetiapine as the internal standard (IS) is described. The analyte and the IS were extracted from human plasma by a simple protein precipitation with methanol and were analyzed by high-performance liquid chromatography coupled to an electrospray tandem triple quadrupole mass spectrometer (HPLC-ESI-MS/MS). Chromatography was performed isocratically on a C(18), 5 µm analytical column and the run time was 1
Biomedical ChromatographyVolume 24, Issue 7, pages 774–781, July 2010
Determination of chlorpheniramine in human plasma by HPLC-ESI-MS/MS: application to a dexchlorpheniramine comparative bioavailability study
Ronilson Agnaldo Moreno, Diogo Oliveira-Silva, Carlos Eduardo Sverdloff, Bruno Carter Borges, Paulo Alexandre Rebelo Galvinas, Rafael Barrientos Astigarraga, Ney Carter Borges
In the present study a fast, sensitive and robust validated method to quantify chlorpheniramine in human plasma using brompheniramine as internal standard (IS) is described. The analyte and the IS were extracted from plasma by LLE (diethyl ether–dichloromethane, 80:20, v/v) and analyzed by HPLC-ESI-MS/MS. Chromatographic separation was performed using a gradient of methanol from 35 to 90% with 2.5 mm NH4OH on a Gemini Phenomenex C8 5 μm column (50 × 4.6 mm i.d.) in 5.0 min/run. The method fitted to a linear calibration curve (0.05–10 ng/mL, R > 0.9991). The precision (%CV) and accuracy ranged, respectively: intra-batch from 1.5 to 6.8% and 99.1 to 106.6%, and inter-batch from 2.4 to 9.0%, and 99.9 to 103.1%. The validated bioanalytical procedure was used to assess the comparative bioavailability in healthy volunteers of two dexchlorpheniramine 2.0 mg tablet formulations (test dexchlorpheniramine, Eurofarma, and reference Celestamine®, Schering-Plough). The study was conducted using an open, randomized, two-period crossover design with a 2 week washout interval. Since the 90% confidence interval for Cmax and AUC ratios were all within the 80–125% interval proposed by ANVISA and FDA, it was concluded that test and reference formulations are bioequivalent concerning the rate and the extent of absorption. Copyright © 2009 John Wiley & Sons, Ltd.
Cyproterone acetate quantification in human plasma by high-performance liquid chromatography coupled to atmospheric pressure photoionization tandem mass spectrometry. Application to a comparative pharmacokinetics study.
Arzneimittelforschung 2009 ;59(7):335-44
Ney Carter Borges, Ana Mazuqueli, Ronilson Agnaldo Moreno, Rafael Barrientos Astigarraga, Carlos Eduardo Sverdloff, Paulo Alexandre Rebelo Galvinas, Maurício Rocha de Magalhães Sampaio, Washington Moreira da Silva
A specific, fast and sensitive high performance liquid chromatography (HPLC) coupled to atmospheric pressure photoionization (APPI) tandem mass spectrometric (LC-MS/MS) assay was developed for the determination of cyproterone (CYP) acetate (CAS 427-51-0) in human plasma. The retention times were 3.26 and 2