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High-throughput Determination of Nonsteroidal Anti-Inflammatory Drugs in Human Plasma by HILIC-MS/MS

High-throughput Determination of Nonsteroidal Anti-Inflammatory Drugs in Human Plasma by HILIC-MS/MS

Tetsuya Nemoto, Xiao-Pen Lee, Takeshi Kumazawa, Chika Hasegawa, Masaya Fujishiro, Akemi Marumo, Yukiko Shouji, Katsunori Inagaki, Keizo Sato

J Pharm Biomed Anal. 2014 Jan;88:71-80.

PMID: 24036363

Abstract:

A simple and sensitive method was developed and validated here for the analysis of thirteen nonsteroidal anti-inflammatory drugs (NSAIDs) in human plasma samples by hydrophilic interaction liquid chromatography (HILIC)-tandem mass spectrometry (MS/MS). A small volume of plasma (20μL) spiked with compounds was diluted with 80μL of 10-mM ammonium acetate followed by a simple protein precipitation with 400μL of acetonitrile. After centrifugation, the clear supernatant extract was directly injected into the HILIC-MS/MS, without any solvent evaporation and reconstitution steps. The chromatographic separation of the NSAIDs was achieved on a Unison UK-Amino HILIC column (50mm×3mm i.d., particle size 3μm) with a linear gradient elution system composed of 10mM ammonium acetate (pH 6.8) and acetonitrile at a flow rate of 0.4mL/min. The mass spectra obtained by HILIC-MS showed base peak ions due to [M+H](+) for indomethacin, oxaprozin, ketoprofen, alminoprofen, zaltoprofen, tiaprofenic acid, pranoprofen, and ketoprofen-d3 and due to [M-H](-) for etodolac, ibuprofen, diclofenac, fenoprofen, loxoprofen, naproxen, and ibuprofen-d3. Recoveries of these thirteen NSAIDs in plasma were 34.8-113% and the lower limits of quantitation were 0.125-1.25μg/mL. The intra- and interday coefficient of variations for all drugs in plasma were less than 14.6%. The data obtained from actual plasma determinations of zaltoprofen, ibuprofen, and diclofenac are also presented.

Chemicals Related in the Paper:

Catalog Number	Product Name	Structure	CAS Number	Price
AP121662144	Ibuprofen-d3		121662-14-4	Price
AP159490558	Ketoprofen-d3		159490-55-8	Price

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