Journal ArticleDOI
Incurred sample reanalysis (ISR): a decisive tool in bioanalytical research
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TLDR
Five troubleshooting cases encountered in the analyses of incurred samples for bioanalytical methods developed in the laboratory for mesalamine, hydrochlorothiazide, clopidogrel, sildenafil and rabeprazole are summarized to help develop more reliable and efficient bio Analytical methods.Abstract:
The AAPS Workshop 2008 on Current Topics in GLP Bioanalysis: Assay Reproducibility for Incurred Samples was the defining moment in establishing incurred sample reanalysis (ISR) as a mandatory exercise in demonstrating assay reproducibility using incurred (study) samples. The importance of ISR can be envisaged from its role in clinical as well as non-clinical studies. Incurred samples can differ significantly in their composition when compared with the calibration standards and quality control samples that are used to validate the developed method. The present article attempts to summarize five troubleshooting cases encountered in the analyses of incurred samples for bioanalytical methods developed in our laboratory for mesalamine, hydrochlorothiazide, clopidogrel, sildenafil and rabeprazole. The issues identified were related to: sample inhomogeneity, sample processing error, impact of buffer pH during sample preparation, instability of metabolite and change in laboratory environment. The steps taken to trace and correct these incidents are discussed with adequate data. These examples will further broaden the scope and emphasize the significance of ISR. We believe this investigation will help to develop more reliable and efficient bioanalytical methods.read more
Citations
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Validated UPLC–MS/MS method for determination of hordenine in rat plasma and its application to pharmacokinetic study
Jianshe Ma,Shuanghu Wang,Xueli Huang,Peiwu Geng,Congcong Wen,Yunfang Zhou,Linsheng Yu,Xianqin Wang +7 more
TL;DR: The method was successfully applied to pharmacokinetic study of hordenine after oral and intravenous administration and the accuracy of the method ranged from 97.0% to 107.7%.
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LC–tandem mass spectrometry method for the simultaneous determination of metformin and sitagliptin in human plasma after ion-pair solid phase extraction
TL;DR: A reversed-phase liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) method was established for simultaneous determination of two oral hypoglycemic drugs metformin and sitagliptin in human plasma and both the drugs were found to be stable under all mandatory storage conditions.
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Mixed-mode solid phase extraction combined with LC-MS/MS for determination of empagliflozin and linagliptin in human plasma
TL;DR: In this paper, a liquid chromatography-tandem mass spectrometry method was developed and validated for the concurrent determination of antidiabetic drugs, empagliflozin and linagliptin in human plasma.
Journal ArticleDOI
LC-MS/MS analysis of metformin, saxagliptin and 5-hydroxy saxagliptin in human plasma and its pharmacokinetic study with a fixed-dose formulation in healthy Indian subjects.
TL;DR: The validated method was successfully applied to a bioequivalence study with a fixed-dose formulation consisting of 5 mg SAXA and 500’mg MET in 18 healthy subjects and the reproducibility of the assay was demonstrated by reanalysis of 87 incurred samples.
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Simultaneous determination of metoprolol and its metabolites, α-hydroxymetoprolol and O-desmethylmetoprolol, in human plasma by liquid chromatography with tandem mass spectrometry: Application to the pharmacokinetics of metoprolol associated with CYP2D6 genotypes
TL;DR: This method was successfully applied to assess the influence of CYP2D6 genotypes on the pharmacokinetics of MET after oral administration of 100 mg to healthy Korean volunteers.
References
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