Incurred Sample Reproducibility: 10 Years of Experiences: Views and Recommendations from the European Bioanalysis Forum

Kall, Morten A.; Michi, Marco; Strate, Barry van der; Freisleben, Achim; Stoellner, Daniela; Timmerman, Philip

doi:10.4155/bio-2018-0194

Cited by 19 publications

(13 citation statements)

References 8 publications

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“…Where young scientists have performed root cause analysis it has been identified as due to insufficient sample stability, analyst error or issues with sample homogeneity. These findings mimic those presented in previous EBF papers surrounding ISR [10].…”

Section: Theme 3: Dbs/microsamplingsupporting

confidence: 90%

Feedback from the Fifth European Bioanalysis Forum Young Scientist Symposium

et al. 2019

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Since 2014, the European Bioanalysis Forum (EBF) organizes a Young Scientist Symposium. The meeting format was created to provide development opportunities for young scientists to engage in international discussions. Creating a peer community of young scientists has been a proven recipe to lower the threshold and promote engagement in this community of young talents. At the same time, the meetings are aimed at stimulating collaboration between the EBF and academia. This manuscript summarizes the discussions at the Fifth EBF Young Scientist Symposium, held in Bologna (Italy) between 20 and 21 March 2019.

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Section: Theme 3: Dbs/microsamplingsupporting

confidence: 90%

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“…UFLC gradient programming was selected over an isocratic method to get well separation between all three analytes. The retention times for Raloxifene, Raloxifene 4-Glucuronide, N 3 3 3 3 3 3 3 3 3 3 3 [18][19][20] , random repeat study sample analysis is required to be performed as the incurred samples. A validated method, which is reproducible and shows satisfactory data of the long-term stability of the drug in the matrix, may not adequately indicate the stability and reproducibility of actual subject samples (incurred samples).…”

Section: Results: Chromatography Retention Times and Lloqmentioning

confidence: 99%

Untitled

2020

IJPSR

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Simultaneous estimation of parent and its metabolite(s) in a single method poses a threat when one has to monitor one mass transition while running the other compound on liquid chromatographymass spectrometer. This would again become critical once interference is observed at the retention time of compound of interest in-spite of its absence in the sample. In this paper, a selective and sensitive liquid chromatography-tandem mass spectrometry method for the simultaneous determination of Raloxifene and its two active metabolites, Raloxifene 4-Glucuronide and Raloxifene 6-Glucuronide in human plasma was developed and validated. The method involves a rapid solid-phase extraction from plasma, followed by reversed-phase chromatography with gradient flow condition and mass spectrometry detection. Validation parameters were selected ranging from 0.016 to 1.187 ng/mL for Raloxifene, 3.073 to 700.558 ng/mL Raloxifene 4-Glucuronide and 0.311 to 124.526 ng/ml for Raloxifene 6-Glucuronide. The mean recovery for Raloxifene, Raloxifene 4-Glucuronide, and Raloxifene 6-Glucuronide found to be 85.10, 86.30 & 87.20%, respectively. The peak concentration of Raloxifene, Raloxifene 4-Glucuronide, and Raloxifene 6-Glucuronide were 0.330 ng/mL, 153.047 ng/mL and 27.744 ng/mL respectively for the reference product, in fasted conditions. INTRODUCTION: Raloxifene is a selective estrogen receptor modulator (SERM) having selective agonist or antagonist activities on tissues responsive to estrogen. In postmenopausal women with osteoporosis, Raloxifene reduces the incidence of vertebral fractures, preserves bone mass, and increases bone mineral density (BMD) 1-3 .

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“…As per recent regulatory recommendations and various publications (Giri et al, 2018;Kall et al, 2018;Vazvaei, 2018), random repeat study sample analysis is required to be performed as incurred sam- and stability is essential to produce reliable study data. In the biostudy, 10% of samples (from the vicinity of time of C max and elimination phase) were randomly selected for incurred samples reanalysis (ISR) for both of the compounds (leucovorin and 5-methyl tetrahydrofolic acid).…”

Section: Incurred Sample Reanalysismentioning

confidence: 99%

Sensitive and rapid simultaneous quantitation of leucovorin and its major active metabolite 5‐methyl‐tetrahydrofolate in human plasma using a liquid chromatography coupled with triple quadruple mass spectrometry

Dubey

2022

Biomedical Chromatography

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Bioanalysis of an endogenous compound such as leucovorin is never an easy task on a liquid chromatography tandem mass spectrometer (LC–MSMS). Unless it is necessary, regulatory guidance discourages working with surrogate matrices for calibration curve standard preparation. Herein, a selective and sensitive liquid chromatography–tandem mass spectrometry method for simultaneous determination of leucovorin and 5‐methyl tetrahydrofolic acid in human plasma was developed and validated. Stable labeled internal standards, i.e. leucovorin D4 and 5‐ methyl tetrahydrofolic acid 13C5, were used as internal standards to track and compensate the parent compounds during processing and extraction from plasma. The method involves a rapid solid‐phase extraction from plasma followed by reverse‐phase gradient chromatography and mass spectrometry detection with a total run time of 5 min. The method was developed and validated from 5 to 2,202 ng/ml for leucovorin and from 5 to 1,300 ng/ml for 5‐methyl tetrahydrofolic acid. The mean recoveries for leucovorin and 5‐methyl tetrahydrofolic acid were 100.4 and 100.9% respectively. The validated method enabled the simultaneous analysis of leucovorin and 5‐methyl tetrahydrofolic acid in samples from clinical pharmacokinetic studies of leucovorin. The peak concentrations of leucovorin and 5‐methyl tetrahydrofolic acid were 651–883 and 518–635 ng/ml, respectively, in fasted and fed conditions. The terminal half‐life values for leucovorin and 5‐methyl tetrahydrofolic acid were 9.3–10.5 and 9.2–17.6 h, respectively.

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Incurred Sample Reproducibility: 10 Years of Experiences: Views and Recommendations from the European Bioanalysis Forum

Cited by 19 publications

References 8 publications

Feedback from the Fifth European Bioanalysis Forum Young Scientist Symposium

Feedback from the Fifth European Bioanalysis Forum Young Scientist Symposium

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Sensitive and rapid simultaneous quantitation of leucovorin and its major active metabolite 5‐methyl‐tetrahydrofolate in human plasma using a liquid chromatography coupled with triple quadruple mass spectrometry

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