Simultaneous determination of five phthalates in white spirits using liquid-liquid extraction followed by gas chromatography-mass spectrometry

Abstract

The aim of this paper is the development of the method for determination of five phthalates in white spirits. Dimethyl phthalate (DMP), di-n-butyl phthalate (DBP), benzyl butyl phthalate (BBP), di-(2-ethylhexyl) phthalate (DEHP) and di-n-octyl phthalate (DOP) were extracted from white spirits by the optimized liquid-liquid extraction (LLE) method. In order to determine the best method for phthalate determination, LLE procedure was optimized by changing the following parameters: the number of extraction repetitions (1-4), the partial removal of ethanol by evaporation from alcoholic samples prior extraction, the type of agitation and the extraction time. Quantification was achieved by gas chromatography-mass spectrometry (GC-MS) with di-n-butyl adipate (DBA) as internal standard. Phthalates were analyzed using a single ion monitoring (SIM) mode and a base ion for each phthalate was chosen (m/z 149 for DBP, BBP, DEHP and DOP and m/z 163 for DMP). The results show that the most effective phthalate extraction with n-hexane as a solvent is achieved with agitation by hand shaking with one-step extraction. Evaporation of ethanol from alcohol drinks provided the increased recovery value for DMP extraction but did not have an impact on the recovery values of DBP, BBP, DEHP and DOP extractions from the samples.