Analytical Sciences

Abstract − Analytical Sciences, 25(7), 865 (2009).

Determination of Phthalates and Adipate in Physiological Saline Solutions by Solid-Phase Microextraction and Gas Chromatography
Marcel Silveira dos SANTOS, Dilma BUDZIAK, Edmar MARTENDAL, and Eduardo CARASEK
Departamento de Química, Universidade Federal de Santa Catarina, Florianópolis, SC 88040-900, Brazil
This study describes an analytical methodology developed for determination of phthalate esters (di-n-butyl, butylbenzyl and di-2-ethylhexyl phthalate) and adipate (di-n-ethylhexyl adipate) by solid-phase microextraction (SPME) and gas chromatography in normal saline solutions and, in bi-distilled water used to reconstitute medicines. An 85-μm-polyacrylate SPME fiber was selected and used in all analyses. The parameters affecting extraction efficiency were simultaneously optimized, firstly by means of a two-level full factorial design including a center point and subsequently through a Doehlert design for two-variables. Satisfactory detection limits in the range of 0.18 to 0.75 μg L−1 and excellent precision, with relative standard deviation values being lower than 15.1% (n = 6), were obtained. Relative sensitivities of between 72.3 and 124.3% were obtained.