Optimization of the derivatization reaction and the solid-phase microextraction conditions using a D-optimal design and three-way calibration in the determination of non-steroidal anti-inflammatory drugs in bovine milk by gas chromatography-mass spectrometry

被引:48
作者
Arroyo, David [1 ]
Ortiz, M. Cruz [1 ]
Sarabia, Luis A. [2 ]
机构
[1] Univ Burgos, Fac Sci, Dept Chem, Burgos 09001, Spain
[2] Univ Burgos, Fac Sci, Dept Math & Computat, Burgos 09001, Spain
关键词
NSAIDs; Milk; SPME; GC/MS; PARAFAC; European Commission Decision; 2002/657/EC; WATER SAMPLES; KETOPROFEN; RESIDUES; EXTRACTION; FLUNIXIN; PARAFAC2; SEWAGE; NSAIDS;
D O I
10.1016/j.chroma.2011.05.010
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
An experimental design optimization is reported of an analytical procedure used in the simultaneous determination of seven non-steroidal anti-inflammatory drugs (NSAIDs) in bovine milk by gas chromatography with mass spectrometry detection (GC-MS). This analytical procedure involves a solid-phase microextraction (SPME) step and an aqueous derivatization procedure of the NSAIDs to ethyl esters in bovine milk. The following NSAIDs are studied: ibuprofen (IBP), naproxen (NPX). ketoprofen (KPF), diclofenac (DCF), flufenamic acid (FLF), tolfenamic acid (TLF) and meclofenamic acid (MCL). Three kinds of SPME fibers - polyacrylate (PA), polydimethylsiloxane/divinylbenzene (PDMS/DVB) and polydimethylsiloxane (PDMS) - are compared to identify the most suitable one for the extraction process, on the basis of two steps: to determine the equilibrium time of each fiber and to select the fiber that provides the best figures-of-merit values calculated with three-way PARAFAC-based calibration models at the equilibrium time. The best results were obtained with the PDMS fiber. Subsequently, 8 experimental factors (related to the derivatization reaction and the SPME) were optimized by means of a D-optimal design that involves only 14 rather than 512 experiments in the complete factorial design. The responses used in the design are the sample mode loadings of the PARAFAC decomposition which are related to the quantity of each NSAID that is extracted in the experiment. Owing to the fact that each analyte is unequivocally identified in the PARAFAC decomposition, a calibration model is not needed for each experimental condition. The procedure fulfils the performance requirements for a confirmatory method established in European Commission Decision 2002/657/EC. (C) 2011 Elsevier B.V. All rights reserved.
引用
收藏
页码:4487 / 4497
页数:11
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