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Liquid chromatographic determination of meloxicam in serum after solid phase extraction

Radia Ouarezki and Moulay-Hassane Guermouche

Laboratoire de chromatographie, Facult√© de Chimie, USTHB, B.P. no32, El-Alia, Bab-Ezzouar, 96100 Alger, Algeria

 

E-mail: hguermouche@gmail.com

Received: 1 November 2009  Revised: 1 January 2010  Accepted: 8 January 2010

Abstract: A liquid chromatographic method for the determination of meloxicam in serum has been developed. The technique includes a solid phase extraction of the serum samples on [poly (divinylbenzeneco-N-vinylpyrrolidone)] as a solid phase extraction sorbent. After conditioning, the cartridge was loaded with 1 mL of acidified serum containing an internal standard. Elution was carried out using 1 mL of water-acetonitrile (φ r = 1: 1) mixture. After evaporation of the eluate to dryness and reconstitution of the residue with 0.1 mL of methanol, the samples were analyzed on a Symmetry C18 column. Mobile phase consisted of 1 % aqueous acetic acid/THF/acetonitrile (φ r = 60: 30: 10) + 0.1 mL of 1-octane sulfonic acid. Detection was carried out using a photodiode array detector. Full validation of the proposed method is provided. Linearity of the method was proven over the range of 0.01–10 φg mL−1 of meloxicam. Meloxicam assay was accurate and reliable with average intra- and inter-day precisions lower than 5.0 % and the intra- and inter-day accuracy higher than 97 %. Limits of detection (LOD) and quantitation (LOQ) found were 0.003 μg mL−1 and 0.01 μg mL−1, respectively. The proposed method was successfully utilized to quantify meloxicam in serum.

Keywords: liquid chromatography - solid phase extraction - photodiode array detector - meloxicam - serum

Full paper is available at www.springerlink.com.

DOI: 10.2478/s11696-010-0031-9

 

Chemical Papers 64 (4) 429–433 (2010)

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