Development and Validation of an UHPLC-MS/MS Assay for the Therapeutic Monitoring of Brivaracetam Plasma Concentrations in Patients with Epilepsy.


Journal

Therapeutic drug monitoring
ISSN: 1536-3694
Titre abrégé: Ther Drug Monit
Pays: United States
ID NLM: 7909660

Informations de publication

Date de publication:
06 2020
Historique:
pubmed: 15 1 2020
medline: 6 5 2021
entrez: 15 1 2020
Statut: ppublish

Résumé

Brivaracetam is an antiepileptic drug used as an add-on therapy for partial-onset seizures in subjects aged 4 years and older. Owing to potential drug interactions and intersubject variability in plasma concentrations, therapeutic monitoring for brivaracetam may be useful. The aim of this study was to develop a simplified method for measuring brivaracetam plasma concentrations applicable to therapeutic drug monitoring in epilepsy. An ultra high-pressure liquid chromatography-tandem mass spectrometry method was developed and validated according to current guidelines for bioanalytical methods. Sample preparation (100 µL) involved only a simple precipitation step by acetonitrile. Brivaracetam-d7 was used as internal standard. The chromatographic analysis was performed by a Synergi Fusion column using 0.1% formic acid in water/acetonitrile as a binary gradient mobile phase, at a flow rate of 0.3 mL/min. Both brivaracetam and the internal standard eluted at 1.01 minutes. This method was applied to measure trough and 1-hour postmorning dose brivaracetam plasma concentrations of 11 patients with epilepsy. The method was validated over a concentration range of 0.10-10 mcg/mL. The mean recovery was 95%. Both intra- and inter-assay imprecision and inaccuracy were <15% for all quality control samples. The lower limit of quantitation and detection was 0.10 and 0.05 mcg/mL, respectively. No interferences or carry-over was observed. Median (25%-75% quartiles) trough and 1-hour postdosing brivaracetam plasma concentrations were 0.61 mcg/mL (0.47-0.83 mcg/mL) and 1.55 mcg/mL (1.24-2.12 mcg/mL), respectively, at a median dose of 80 mg/d (50-150 mg/d). Large, up to 8-fold, intrasubject fluctuations of brivaracetam concentrations between trough and 1-hour postdosing were observed. The present assay is faster and simpler than previously published analytical reports for brivaracetam in human plasma and is suitable for therapeutic drug monitoring.

Sections du résumé

BACKGROUND
Brivaracetam is an antiepileptic drug used as an add-on therapy for partial-onset seizures in subjects aged 4 years and older. Owing to potential drug interactions and intersubject variability in plasma concentrations, therapeutic monitoring for brivaracetam may be useful. The aim of this study was to develop a simplified method for measuring brivaracetam plasma concentrations applicable to therapeutic drug monitoring in epilepsy.
METHODS
An ultra high-pressure liquid chromatography-tandem mass spectrometry method was developed and validated according to current guidelines for bioanalytical methods. Sample preparation (100 µL) involved only a simple precipitation step by acetonitrile. Brivaracetam-d7 was used as internal standard. The chromatographic analysis was performed by a Synergi Fusion column using 0.1% formic acid in water/acetonitrile as a binary gradient mobile phase, at a flow rate of 0.3 mL/min. Both brivaracetam and the internal standard eluted at 1.01 minutes. This method was applied to measure trough and 1-hour postmorning dose brivaracetam plasma concentrations of 11 patients with epilepsy.
RESULTS
The method was validated over a concentration range of 0.10-10 mcg/mL. The mean recovery was 95%. Both intra- and inter-assay imprecision and inaccuracy were <15% for all quality control samples. The lower limit of quantitation and detection was 0.10 and 0.05 mcg/mL, respectively. No interferences or carry-over was observed. Median (25%-75% quartiles) trough and 1-hour postdosing brivaracetam plasma concentrations were 0.61 mcg/mL (0.47-0.83 mcg/mL) and 1.55 mcg/mL (1.24-2.12 mcg/mL), respectively, at a median dose of 80 mg/d (50-150 mg/d). Large, up to 8-fold, intrasubject fluctuations of brivaracetam concentrations between trough and 1-hour postdosing were observed.
CONCLUSIONS
The present assay is faster and simpler than previously published analytical reports for brivaracetam in human plasma and is suitable for therapeutic drug monitoring.

Identifiants

pubmed: 31934942
doi: 10.1097/FTD.0000000000000726
pii: 00007691-202006000-00015
doi:

Substances chimiques

Anticonvulsants 0
Pyrrolidinones 0
brivaracetam U863JGG2IA

Types de publication

Journal Article Research Support, Non-U.S. Gov't

Langues

eng

Sous-ensembles de citation

IM

Pagination

445-451

Références

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Schoemaker R, Wade JR, Stockis A. Brivaracetam population pharmacokinetics and exposure- response modeling in adult subjects with partial-onset seizures. J Clin Pharmacol. 2016;56:1591–1602.
Stockis A, Watanabe S, Scheen A, et al. Effect of rifampin on the disposition of brivaracetam in human subjects: further insights into brivaracetam hydrolysis. Drug Metab Dispos. 2016;44:792–799.
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Liu E, Dilley D, McDonough B, et al. Safety and tolerability of adjunctive brivaracetam in pediatric patients <16 years with epilepsy: an open-label trial. Paediatr Drugs. 2019;21:291–301.
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Iqbal M, Khalil NY, Ezzeldin E, et al. Simultaneous detection and quantification of three novel prescription drugs of abuse (Suvorexant, Lorcaserin and Brivaracetam) in human plasma by UPLC-MS-MS. J Anal Toxicol. 2019;43:203–211.
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EMEA/CHMP/EWP/192217/2009. Committee for Medicinal Products for Human Use (CHMP), Guideline on Bioanalytical Method Validation. 2011:1–22. Available at: http://www.ema.europa.eu/docs/en_GB/document_library/Scientific_guideline/2011/08/WC500109686.pdf. Accessed October 30, 2019.
International Conference on Harmonisation. ICH Harmonised Tripartite Guideline Prepared within the Third International Conference on Harmonisation of Technical Requirements for the Registration of Pharmaceuticals for Human Use (ICH), Validation of Analytical Procedures: Methodology. 1996:1–13. Available at: https://www.ema.europa.eu/en/documents/scientific-guideline/ich-q-2-r1-validation-analytical-procedures-text-methodology-step-5_en.pdf. Accessed October 30, 2019.
Vander Heyden Y, Nijhuis A, Smeyers-Verbeke J, et al. Guidance for rubustness/ruggedness tests in method validation. J Pharm Biomed Anal. 2001;24:723–753.
Klein P, Diaz A, Gasalla T, et al. A review of the pharmacology and clinical efficacy of brivaracetam. Clin Pharmacol. 2018;10:1–22.
Hiemke C, Bergemann N, Clement HW, et al. Consensus guidelines for therapeutic drug monitoring in neuropsychopharmacology: update 2017. Pharmacopsychiatry. 2018;51:9–62.
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Auteurs

Susan Mohamed (S)

IRCCS-Istituto delle Scienze Neurologiche di Bologna; and.

Roberto Riva (R)

IRCCS-Istituto delle Scienze Neurologiche di Bologna; and.
Department of Biomedical and Neuromotor Sciences, University of Bologna, Bologna, Italy.

Manuela Contin (M)

IRCCS-Istituto delle Scienze Neurologiche di Bologna; and.
Department of Biomedical and Neuromotor Sciences, University of Bologna, Bologna, Italy.

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Classifications MeSH