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Determination of nabumetone and 6-methoxy-2-naphthylacetic acid in plasma using HPLC with UV and MS detection


Authors: Lenka Nespěšná 1,2;  Martin Štícha 1;  Olga Matoušková 2;  František Perlík 2;  Ondřej Slanař 2
Authors‘ workplace: Univerzita Karlova v Praze, Katedra organické a jaderné chemie, Přírodovědecká fakulta 1;  Univerzita Karlova v Praze, Farmakologický ústav 1. lékařské fakulty 2
Published in: Čes. slov. Farm., 2011; 60, 17-24
Category: Original Articles

Overview

The study aimed to establish and validate an analytical method for the determination of nabumetone and 6-methoxy-2-naphthylacetic acid (6-MNA) in human plasma after a single therapeutic dose of the drug. Two methods based on HPLC with UV and MS detection were compared. Optimal results in sample preparation were achieved using solid phase extraction. The recovery reached approximately 84% and 86–90% for nabumetone and 6-MNA, respectively. A reverse C18 column was used for HPLC separation of the analytes. The limit of UV detection was 50 nM and 0.1 μM for 6-MNA and nabumetone, respectively. The limit of MS detection was 1 μM and 0.5 μM for 6‑MNA and nabumetone, respectively. Precision ranged between 4.2–14.4% and 4.6–8.5% using UV and MS detection for nabumetone, respectively. The respective values for 6-MNA were 2.4–12.5% and 2.1–9.4%. Accuracy ranged between 93.4–109.6% in UV detection and 86.2–107.9% using UV and MS detection for nabumetone, respectively. The respective values for 6-MNA were 87.8–107.4% and 86.3–106.4%. The method was subsequently applied to determine the pharmacokinetic parameters of nabumetone and 6-MNA in a group of 24 healthy volunteers.

Key words:
nabumetone – pharmacokinetics – 6-methoxy-2-naphthylacetic acid – HPLC – LC/MS


Sources

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