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J Chromatogr A. 2016 Nov 25;1474:1-7. doi: 10.1016/j.chroma.2016.10.058. Epub 2016 Oct 25.

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

Author information

1
Department of Agriculture, Environment and Food, University of Molise, via De Sanctis, I-86100 Campobasso, Italy. Electronic address: mvrusso@unimol.it.
2
DIT, INAIL Research Area, via Roberto Ferruzzi 38/40, I-00143 Rome, Italy.
3
Department of Agriculture, Environment and Food, University of Molise, via De Sanctis, I-86100 Campobasso, Italy.

Abstract

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 0.1g product sample and addition of anthracene as Internal Standard, 250μL of n-heptane are used as extraction solvent. The solution, held for 5min 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 4000rpm for 30min. About 100μL of heptane are recovered and 1μL 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 20ngg-1, respectively, for all the PAEs except for iBcEP (23 and 43ngg-1, respectively). The linear dynamic range of this procedure is between 10 and 5000ngg-1 with R2 ≥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 (14ngg-1), DBP (11ngg-1) and DEHP (64ngg-1).

KEYWORDS:

Baby food; DLLME; Endocrine disruptor; Freeze-dried; GC-IT/MS; Phthalate esters

PMID:
28314431
DOI:
10.1016/j.chroma.2016.10.058
[Indexed for MEDLINE]

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