Open AccessDetermination of Phthalates and Adipate in Physiological Saline Solutions by Solid-Phase Microextraction and Gas Chromatography
Author(s) -
Mercedes Santos,
Dilma Budziak,
Edmar Martendal,
Eduardo Carasek
Publication year - 2009
Publication title -
analytical sciences
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.392
H-Index - 73
eISSN - 1348-2246
pISSN - 0910-6340
DOI - 10.2116/analsci.25.865
Subject(s) - chemistry , adipate , chromatography , solid phase microextraction , phthalate , repeatability , factorial experiment , gas chromatography , extraction (chemistry) , detection limit , gas chromatography–mass spectrometry , mass spectrometry , organic chemistry , statistics , mathematics , polymer chemistry
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-microm-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 microg 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.