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Solid‐phase microextraction with gas chromatography and mass spectrometry determination of benzo(a)pyrene in microcrystalline waxes used as food additives
Author(s) -
Conchione Chiara,
Purcaro Giorgia,
Conte Lanfranco S.,
Moret Sabrina
Publication year - 2015
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.201401246
Subject(s) - chemistry , chromatography , solid phase microextraction , mass spectrometry , gas chromatography , wax , pyrene , gas chromatography–mass spectrometry , benzo(a)pyrene , microcrystalline , benzopyrene , organic chemistry , crystallography
Microcrystalline waxes are mixtures of solid, saturated hydrocarbons mainly branched and characterized by a carbon number over C 60 . They are used as food additives for the surface treatment of confectionery and some fruit varieties, in chewing gum base, protective coatings, defoaming agents, and surface finishing agents. Commission Regulation No 231/2012 established physical and chemical specifications for microcrystalline waxes to use in food, and posed a limit of 50 μg/kg for benzo(a)pyrene. Due to the low solubility of microcrystalline waxes in organic solvents and matrix interferences, analytical determination of benzo(a)pyrene represents a difficult task. The official method for indirect determination of total polycyclic aromatic hydrocarbons uses unspecific spectrophotometric detection and a quite laborious, time‐ and solvent‐consuming extraction method. A liquid–liquid partition method followed by solid‐phase microextraction was developed to isolate benzo(a)pyrene from the bulk of saturated hydrocarbons in microcrystalline waxes, with the aim to have a simple and effective method to verify compliance with the legal limit. The final determination was carried out by gas chromatography coupled to mass spectrometry. Good linearity was obtained, along with a recovery of about 80% from the liquid–liquid partitions. The repeatability of the entire method was <6% and accuracy was <3%.