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  • High-throughput LC-MS/MS assay for 6-methoxy-2-naphthylacetic acid, an active metabolite of nabumetone in human plasma and its application to bioequivalence study.

High-throughput LC-MS/MS assay for 6-methoxy-2-naphthylacetic acid, an active metabolite of nabumetone in human plasma and its application to bioequivalence study.

Biomedical chromatography : BMC (2008-07-25)
Bhavin N Patel, Naveen Sharma, Mallika Sanyal, Arpana Prasad, Pranav S Shrivastav
ABSTRACT

A simple, precise and accurate assay for the determination of 6-methoxy-2-naphthylacetic acid (6-MNA), an active metabolite of nabumetone in human plasma, was developed and validated using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The analyte (6-MNA) and propranolol (internal standard, IS) were extracted from 200 microL aliquot of human plasma via solid-phase extraction employing HLB Oasis cartridges and separated on a Discovery HS C18 (50 x 4.6 mm, 5 microm) column. Detection of analyte and IS was done by tandem mass spectrometry with a turbo ion spray interface operating in positive ion and multiple reaction monitoring acquisition mode. The total chromatographic runtime was 3.0 min with retention time for 6-MNA and IS at 1.97 and 1.26 min, respectively. The method was validated over a dynamic linear range of 0.20-60.00 microg/mL for 6-MNA with mean correlation coefficient r > or = 0.9986. The intra-batch and inter-batch precision (%CV) across five validation runs (lower limit of quantiation, low-, medium- and high-quality controls and upper limit of quantitation) was less than 7.5%. The accuracy determined at these levels was within -5.8 to +0.2% in terms of percentage bias. The method was successfully applied for a bioequivalence study of 750 mg nabumetone tablet formulation in 12 healthy Indian male subjects under fasted condition.

MATERIALS
Product Number
Brand
Product Description

Supelco
Discovery® HS C18 Prep Guard Cartridge, 10 μm particle size, L × I.D. 1 cm × 21.2 mm
Supelco
Discovery® HS C18 HPLC Column, 5 μm particle size, L × I.D. 10 cm × 2.1 mm
Supelco
Discovery® HS C18 HPLC Column, 5 μm particle size, L × I.D. 25 cm × 10 mm
Supelco
Discovery® HS C18 HPLC Column, 5 μm particle size, L × I.D. 5 cm × 4.6 mm
Supelco
Discovery® HS C18 HPLC Column, 5 μm particle size, L × I.D. 15 cm × 4 mm
Supelco
Discovery® HS C18 HPLC Column, 5 μm particle size, L × I.D. 25 cm × 4 mm
Supelco
Discovery® HS C18 HPLC Column, 5 μm particle size, L × I.D. 10 cm × 4.6 mm
Supelco
Discovery® HS C18 HPLC Column, 10 μm particle size, L × I.D. 25 cm × 21.2 mm
Supelco
Discovery® HS C18 HPLC Column, 5 μm particle size, L × I.D. 25 cm × 21.2 mm
Supelco
Discovery® HS C18 HPLC Column, 5 μm particle size, L × I.D. 5 cm × 2.1 mm
Supelco
Discovery® HS C18 HPLC Column, 5 μm particle size, L × I.D. 15 cm × 2.1 mm
Supelco
Discovery® HS C18 HPLC Column, 5 μm particle size, L × I.D. 25 cm × 4.6 mm
Supelco
Discovery® HS C18 HPLC Column, 5 μm particle size, L × I.D. 15 cm × 4.6 mm
Supelco
Nabumetone, analytical standard
Supelco
Discovery® HS C18 HPLC Column, 3 μm particle size, L × I.D. 5 cm × 4.6 mm
Supelco
Discovery® HS C18 HPLC Column, 3 μm particle size, L × I.D. 15 cm × 2.1 mm
Supelco
Discovery® HS C18 HPLC Column, 3 μm particle size, L × I.D. 7.5 cm × 2.1 mm
Nabumetone, European Pharmacopoeia (EP) Reference Standard
Supelco
Discovery® HS C18 HPLC Column, 3 μm particle size, L × I.D. 5 cm × 2.1 mm
Supelco
Discovery® HS C18 HPLC Column, 3 μm particle size, L × I.D. 15 cm × 4.6 mm
Supelco
Discovery® HS C18 HPLC Column, 3 μm particle size, L × I.D. 7.5 cm × 4.6 mm