Determination of acidic drugs in sewage water by gas chromatography-mass spectrometry as tert.-butyldimethylsilyl derivatives

被引：146

作者：

Rodríguez, I ^{[1
]}

Quintana, JB ^{[1
]}

Carpinteiro, J ^{[1
]}

Carro, AM ^{[1
]}

Lorenzo, RA ^{[1
]}

Cela, R ^{[1
]}

机构：

[1] Univ Santiago de Compostela, Dept Quim Analit Nutr & Bromatol, Santiago De Compostela 15782, Spain

来源：

JOURNAL OF CHROMATOGRAPHY A | 2003年 / 985卷 / 1-2期

关键词：

water analysis; derivatization; GC; non-steroidal anti-inflammatory drugs;

D O I：

10.1016/S0021-9673(02)01528-5

中图分类号：

Q5 [生物化学];

学科分类号：

071010 ; 081704 ;

摘要：

A procedure is described for the determination of five acidic non-steroidal anti-inflammatory pharmaceuticals (ibuprofen, naproxen, ketoprofen, tolfenamic acid and diclofenac) in sewage water. The analytical method involves the concentration of water samples using a solid-phase extraction polymeric sorbent, functionalized with N-vinylpyrrolidone. Analytes were eluted with ethyl acetate, derivatized using N-methyl-N-(tert.-butyldimethylsilyl)trifluoroacetamide (MTBSTFA) and analyzed by GC-MS. Influence of time, temperature and volume of MTBSTFA in the yield of the derivatization step were studied in detail using a factorial central composite design. Quantification limits of the analytical procedure for 500 ml of sewage water ranged from 20 to 50 ng/l. Recoveries from 90 to 115% were found for sewage water samples spiked with the studied compounds at the low ng/ml level. Results obtained for real samples show the presence of ibuprofen and naproxen in both influent and effluent of a sewage water treatment plant. (C) 2002 Elsevier Science B.V. All rights reserved.

引用

页码：265 / 274

页数：10

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