RESUMO
A screw-based portable and simple solid phase microextraction device was fabricated by a 3D printer and used in combination with the developed silver-incorporated porous polyaniline film pencil lead solid-phase microextraction fiber (Ag/PANI SPME). Scanning electron microscopy revealed a porous structure of the electrodeposited Ag/PANI film. The spectrum from energy dispersive x-ray spectroscopy (EDS) and the elemental map confirmed the presence of silver in the porous polymer film. It was used under stirring for the extraction of five phthalate esters: dimethyl phthalate (DMP), diethyl phthalate (DEP), dibutyl phthalate (DBP), benzyl butyl phthalate (BBP) and di-2-ethylhexyl phthalate (DEHP). The extracted solution was identified and quantified by gas chromatography using a flame ionization detector (GC-FID). Under the optimum conditions of the developed method, a good linearity was obtained in a concentration range of 5.0-1000⯵gâ¯L-1 for all five phthalate esters with limits of detection (LODs) of 4.41⯱â¯0.91⯵gâ¯L-1, 3.98⯱â¯0.92⯵gâ¯L-1, 3.65⯱â¯0.74⯵gâ¯L-1, 4.91⯱â¯0.52⯵gâ¯L-1 and 4.25⯱â¯0.66⯵gâ¯L-1 for DMP, DEP, DBP, BBP and DEHP, respectively. The developed method provided good precision when tested with standard solutions (RSDâ¯<â¯5.5%, nâ¯=â¯6) and real samples (RSDâ¯<â¯3.4%, nâ¯=â¯6). Good fiber-to-fiber reproducibility was also confirmed by extraction with six newly prepared fibers; recoveries ranged from 81.09⯱â¯0.54% to 92.92⯱â¯0.46% with RSD <6.6%. The developed method was used to determine phthalate esters in 14 cosmeceutical samples. In rubbing alcohol samples, DEP and DEHP were detected at 7.03⯱â¯0.76⯵gâ¯L-1 and 5.89⯱â¯0.53⯵gâ¯L-1, respectively, while in contact lens cleaners, DEHP was found in a concentration range from 5.3⯱â¯1.1⯵gâ¯L-1 to 6.8⯱â¯1.2⯵gâ¯L-1. No phthalate esters contamination was detectable in saline solutions, eye cleaners and antibacterial disinfectant liquids. Recoveries in the range of 81.92⯱â¯0.99% to 102.4⯱â¯1.1% indicated the good accuracy of the developed method.
