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  • Development and validation of a GC/MS method for the simultaneous determination of levetiracetam and lamotrigine in whole blood.

Development and validation of a GC/MS method for the simultaneous determination of levetiracetam and lamotrigine in whole blood.

Journal of pharmaceutical and biomedical analysis (2014-09-23)
Panagiota Nikolaou, Ioannis Papoutsis, Artemisia Dona, Chara Spiliopoulou, Sotiris Athanaselis
ABSTRACT

A sensitive and accurate gas chromatography-mass spectrometric method was developed and validated for the simultaneous determination of levetiracetam and lamotrigine in whole blood. A solid-phase extraction (SPE) procedure using HF Bond Elut C18 columns followed by derivatization using N-methyl-N-tert-butyldimethylsilyl-trifluoroacetamide (MTBSTFA) with 1% tert-butyldimethylsilyl chloride (TBDMSCl) was used. In this assay, levetiracetam-d6 was used as internal standard. Limits of detection and quantification were 0.15 and 0.50 μg/mL, respectively, for both analytes. The method was proved to be linear within the concentration range of 0.50-50.0 μg/mL (R(2) ≥ 0.992) for both analytes. Absolute recovery was found to be at least 90.0 and 97.2% for levetiracetam and lamotrigine, respectively. Intra-day and inter-day accuracy values for both analytes were ranged from -6.5 to 4.2 and -6.6 to 3.0%, respectively, whereas their respective precision values were less than 11.4 and 8.3%. The developed method was successfully used in our laboratory for quantification of levetiracetam and lamotrigine blood concentrations during the investigation of forensic cases where these antiepileptic drugs were involved. This method could also be used for therapeutic drug monitoring purposes.

MATERIALS
Product Number
Brand
Product Description

Supelco
N,O-Bis(trimethylsilyl)trifluoroacetamide with trimethylchlorosilane, with 1% trimethylchlorosilane, derivatization grade (GC derivatization), LiChropur
Sigma-Aldrich
Chlorotrimethylsilane, Wacker Chemie AG, ≥99.0% (GC)
Supelco
Trifluoroacetic anhydride, derivatization grade (GC derivatization), LiChropur, ≥99.0% (GC)
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Chlorotrimethylsilane, ≥98.0% (GC)
Sigma-Aldrich
Chlorotrimethylsilane, puriss., ≥99.0% (GC)
Supelco
N,O-Bis(trimethylsilyl)trifluoroacetamide with trimethylchlorosilane, derivatization grade (GC derivatization), LiChropur, contains 10% TMCS, 98% (excluding TMCS)
Sigma-Aldrich
N-tert-Butyldimethylsilyl-N-methyltrifluoroacetamide with 1% tert-Butyldimethylchlorosilane, ≥95%
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tert-Butylchlorodimethylsilane solution, 50 wt. % in toluene
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Chlorotrimethylsilane, purified by redistillation, ≥99%
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Trifluoroacetic anhydride, ReagentPlus®, ≥99%
Supelco
N-tert-Butyldimethylsilyl-N-methyltrifluoroacetamide with 1% tert-Butyldimethylchlorosilane, LiChropur, ≥95.0% (GC)
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Chlorotrimethylsilane, derivatization grade (GC derivatization), LiChropur, ≥99.0% (GC)
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Methanol, HPLC Plus, ≥99.9%
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Methanol, Laboratory Reagent, ≥99.6%
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Methanol, suitable for HPLC, gradient grade, suitable as ACS-grade LC reagent, ≥99.9%
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Methanol, suitable for HPLC, gradient grade, ≥99.9%
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Methanol, ACS spectrophotometric grade, ≥99.9%
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Residual Solvent - Acetonitrile(solution in DMSO), Pharmaceutical Secondary Standard; Certified Reference Material
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Methanol, Pharmaceutical Secondary Standard; Certified Reference Material
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Acetonitrile(Neat), Pharmaceutical Secondary Standard; Certified Reference Material
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Heptafluorobutyric anhydride, derivatization grade (GC derivatization), LiChropur, ≥99.0%
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Isopropyl alcohol, ≥99.7%, FCC, FG
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Heptafluorobutyric anhydride, ≥98%
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Methanol, purification grade, 99.8%
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Methanol, suitable for NMR (reference standard)
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Heptafluorobutyric anhydride, derivatization grade (GC derivatization), LiChropur, ≥99.0%
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Methanol, anhydrous, 99.8%
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Methanol, analytical standard
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Methanol, ACS reagent, ≥99.8%