PMID- 20602942 OWN - NLM STAT- MEDLINE DCOM- 20101116 LR - 20131121 IS - 1873-3573 (Electronic) IS - 0039-9140 (Linking) VI - 82 IP - 2 DP - 2010 Jul 15 TI - The role of the acquisition methods in the analysis of the non-steroidal anti-inflammatory drugs in Danube River by gas chromatography-mass spectrometry. PG - 600-7 LID - 10.1016/j.talanta.2010.05.014 [doi] AB - In this paper authors describe a GC-MS acquisition study, relating to the most common, non-steroidal anti-inflammatory drugs (NSAIDs), such as ibuprofen, naproxen, ketoprofen and diclofenac. As novelties to the field, for the trimethylsilyl (TMS) oxime ester derivatives of NSAIDs, at first, a tandem mass spectrometric (MS/MS) acquisition method has been developed, and, also for the first time, the three acquisition techniques, the full scan (FS), the selective ion monitoring (SIM) and the currently optimized MS/MS ones, have been compared: all three in parallel, under strictly the same derivatization/instrumental conditions, both from model solutions and from the Danube River samples. Critical evaluation of the three acquisition protocols was collated on their analytical performances and validated with the same characteristics like the six point calibration curve, the relative standard deviation percentages (RSD%) of parallel tests, the limit of quantitation (LOQ) and the instrumental limit of quantitation (ILQ) values. Data of six point calibration (r(2)>or=0.997) and RSD% (average: 5.8 RSD%) values proved to be independent on the acquisition methods, while, LOQ and ILQ values furnished considerable differences. Decreasing LOQ data, (expressed in ng/L concentrations) were obtained in the FS, SIM, MS/MS line for ibuprofen (1.0, 0.43, 0.41), naproxen (1.1, 1.0, 0.42), ketoprofen (2.6, 1.0, 0.49) and diclofenac (1.4, 0.41, 0.21), respectively. The same trend was determined in terms of the ILQ values. The practical utility of the optimized MS/MS technique was confirmed by the quantitation of the NSAID contents of the Danube River samples, determined by all three acquisition techniques. Results obtained confirmed the primary importance of the MS/MS acquisition method, even in comparison to the SIM one: avoiding the extreme overestimation of the ibuprofen (approximately 100%) and ketoprofen (approximately 400%) concentrations in the Danube River samples. CI - Copyright 2010 Elsevier B.V. All rights reserved. FAU - Helenkar, A AU - Helenkar A AD - Institute of Chemistry Department of Analytical Chemistry, L. Eotvos University, Budapest, Hungary. FAU - Sebok, A AU - Sebok A FAU - Zaray, Gy AU - Zaray G FAU - Molnar-Perl, I AU - Molnar-Perl I FAU - Vasanits-Zsigrai, A AU - Vasanits-Zsigrai A LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20100611 PL - Netherlands TA - Talanta JT - Talanta JID - 2984816R RN - 0 (Anti-Inflammatory Agents, Non-Steroidal) RN - 0 (Water Pollutants, Chemical) RN - 144O8QL0L1 (Diclofenac) RN - 57Y76R9ATQ (Naproxen) RN - 90Y4QC304K (Ketoprofen) RN - WK2XYI10QM (Ibuprofen) SB - IM MH - Anti-Inflammatory Agents, Non-Steroidal/*analysis/chemistry MH - Diclofenac/analysis MH - Gas Chromatography-Mass Spectrometry/*methods MH - Ibuprofen/analysis MH - Ketoprofen/analysis MH - Limit of Detection MH - Naproxen/analysis MH - Rivers/*chemistry MH - Water Pollutants, Chemical/analysis EDAT- 2010/07/07 06:00 MHDA- 2010/11/17 06:00 CRDT- 2010/07/07 06:00 PHST- 2010/01/19 00:00 [received] PHST- 2010/04/28 00:00 [revised] PHST- 2010/05/10 00:00 [accepted] PHST- 2010/07/07 06:00 [entrez] PHST- 2010/07/07 06:00 [pubmed] PHST- 2010/11/17 06:00 [medline] AID - S0039-9140(10)00354-1 [pii] AID - 10.1016/j.talanta.2010.05.014 [doi] PST - ppublish SO - Talanta. 2010 Jul 15;82(2):600-7. doi: 10.1016/j.talanta.2010.05.014. Epub 2010 Jun 11.