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3rd meeting of young researchers at UP 1 - IJUP - Universidade do ...

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Effect <strong>of</strong> dimethyldioctadecylammonium bromide on the<br />

potenciometric determin<strong>at</strong>ion <strong>of</strong> sulfamethoxazole<br />

S. A.A. Almeida 1,2,3 , M.C.B.S.M.Montenegro 2 and M.G.F. Sales 3<br />

1 REQUIMTE/<strong>Universidade</strong> <strong>do</strong> Porto, ISEP, Instituto Superior de Engenharia <strong>do</strong> Porto, Portugal.<br />

2 INSA-Porto, Instituto Nacional de Saúde Dr. Ricar<strong>do</strong> Jorge-Porto, Portugal.<br />

3 REQUIMTE/Serviço de Química-Física, Faculdade de Farmácia da <strong>Universidade</strong> <strong>do</strong> Porto, Portugal<br />

Sulfamethoxazole, 4-Amino-N-(5-methyl-3-isoxazolyl)benzenesulfonamide (SMX), is an<br />

effective antimicrobial agent in tre<strong>at</strong>ing infections caused by Streptococcus, Staphylococcus,<br />

Salmonella, and Coccidia [1]. It acts as a competitive antagonist <strong>of</strong> p-aminobenzoic acid<br />

(PABA) and thus as an inhibitor <strong>of</strong> folic acid synthesis, since PABA is an integral component<br />

<strong>of</strong> the structure <strong>of</strong> folic acid [2]. It is used for human and veterinary purposes and may be<br />

found in the aqu<strong>at</strong>ic environment as a contaminant.<br />

The determin<strong>at</strong>ion <strong>of</strong> SMX may be carried out by means <strong>of</strong> several analytical techniques, such<br />

as potentiometry with PVC-based ion selective electrodes (ISEs). Some important fe<strong>at</strong>ures <strong>of</strong><br />

the PVC-based membranes, such as the ionophore and the amount/kind <strong>of</strong> additive used,<br />

influence significantly the analytical performance <strong>of</strong> ISEs. Hence, in this work SMX selective<br />

electrodes were prepared with alpha-cyclodextrins (α−CD) and with or without additive<br />

dimethyldioctadecylammonium bromide (DDABr).<br />

A Crison ® µpH 2002 decimilivoltammeter (±0.1 mV sensitivity) was used for measuring the<br />

potential differences between an Orion 90-02-00 <strong>do</strong>uble junction AgCl/Ag reference electrode<br />

and the indic<strong>at</strong>ing electrode. The selective electrodes had no internal reference solution and<br />

used an epoxy-graphite m<strong>at</strong>rix as conductive solid contact [3]. Calibr<strong>at</strong>ion curves followed the<br />

Litre beaker method [4]. All electrodes were placed in a convenient support over a magnetic<br />

stirrer and immersed in 50.00 ml <strong>of</strong> HEPES 0.01 M. Suitable increments <strong>of</strong> SMX standard<br />

solution were added.<br />

ISEs without additive did not display a potentiometric response, but electrodes with 25% <strong>of</strong><br />

DDABr presented sensitivities <strong>of</strong> 57 mV/decade, close to those <strong>of</strong> the Nernst equ<strong>at</strong>ion. A slight<br />

increase in slope was also observed for an increasing amount <strong>of</strong> additive. Both limit <strong>of</strong><br />

detection (LOD) and lower limit <strong>of</strong> linear range (LLLR) remained unaffected by the additive<br />

amount.<br />

References:<br />

[1] JJ. Flórez, J.A. Armijo and A. Mediavilla (1999), Farmacología Humana, Masson (Ed.), <strong>3rd</strong> ed.,<br />

Spain, pp. 1151–1153.<br />

[2] R.F. Bevill (1988), Veterinary Pharmacology and Therapeutics, in: N.H. Booth and L. McDonald,<br />

Editors Iowa University Press, Ames, IA, 48.<br />

[3] Lapa RAS, Lima JLFC and Silva AMR (1990), Construction <strong>of</strong> calcium ion-selective electrodes<br />

without inner reference solution - an applic<strong>at</strong>ion to calcium and magnesium determin<strong>at</strong>ions in<br />

parenteral and hemodialysis solution. Il Fármaco, 45, pp.901–913.<br />

[4] Buck RP, Cos<strong>of</strong>ret VV (1993), Recommended procedures for calibr<strong>at</strong>ion <strong>of</strong> ion-selective electrodes.<br />

Pure Appl. Chem., 65,pp. 1849–1858.<br />

3 rd <strong>meeting</strong> <strong>of</strong> <strong>young</strong> <strong>researchers</strong> <strong>at</strong> <strong>UP</strong> 243

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