Fast analysis of phthalates in freeze-dried baby foods by ultrasound-vortex-assisted liquid-liquid microextraction coupled with gas chromatography-ion trap/mass spectrometry

This paper is focused on the determination of phthalates (PAEs), compounds plausibly endocrine disruptors, in baby food products by means of a method based on ultrasound-vortex-assisted liquid-liquid microextraction coupled with GC-IT/MS (UVALLME-GC-IT/MS). Particularly, the whole procedure allows the determination of six phthalates such as DMP, DEP, DBP, iBcEP, BBP and DEHP. After dissolution of 0.1 g product sample and addition of anthracene as Internal Standard, 250 mu L of n-heptane are used as extraction solvent. The solution, held for 5 min on the vortex mixer and for 6min in an ultrasonic bath at 100W for favoring the solvent dispersion and consequently the analyte extraction, is centrifuged at 4000 rpm for 30 min. About 100 mu L of heptane are recovered and 1 mu L is injected into the GC-IT/MS. All the analytical parameters investigated are deeply discussed: under the best conditions, the percentage recoveries range between 96.2 and 109.2% with an RSD <= 10.5% whereas the Limit of Detections (LODs) and the Limit of Quantifications (LOQs) are below 11 and 20 ng g(-1), respectively, for all the PAEs except for iBcEP (23 and 43 ng g(-1), respectively). The linear dynamic range of this procedure is between 10 and 5000 ng g(-1) with R-2 >= 0.92. The method has been applied to real commercial freeze-dried samples (chicken and turkey meats) available on the Italian pharmaceutical market: three PAEs were preliminary identified, i.e. DEP (14 ng g(-1)), DBP (11 ng g(-1)) and DEHP (64 ng g(-1)). (C) 2016 Published by Elsevier B.V.