Skip to Content
Merck
  • Direct-immersion solid-phase microextraction coupled to fast gas chromatography mass spectrometry as a purification step for polycyclic aromatic hydrocarbons determination in olive oil.

Direct-immersion solid-phase microextraction coupled to fast gas chromatography mass spectrometry as a purification step for polycyclic aromatic hydrocarbons determination in olive oil.

Journal of chromatography. A (2013-08-07)
Giorgia Purcaro, Massimo Picardo, Laura Barp, Sabrina Moret, Lanfranco S Conte
ABSTRACT

The aim of the present work was to optimize a preparation step for polycyclic aromatic hydrocarbons in a fatty extract. Solid-phase microextraction is an easy preparation technique, which allows to minimize solvent consumption and reduce sample manipulation. A Carbopack Z/polydimethylsiloxane fiber, particularly suitable for extraction of planar compounds, was employed to extract polycyclic aromatic hydrocarbons from a hexane solution obtained after a previous extraction with acetonitrile from oil, followed by a liquid-liquid partition between acetonitrile and hexane. The proposed method was a rapid and sensitive solution to reduce the interference of triglycerides saving the column life and avoiding frequent cleaning of the mass spectrometer ion source. Despite the non-quantitative extraction of polycyclic aromatic hydrocarbons from oil using acetonitrile, the signal-to-noise ratio was significantly improved obtaining a limit of detection largely below the performance criteria required by the European Union legislation.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Zirconium, powder, −100 mesh
Supelco
Carbopack Adsorbent, matrix Carbopack X, 60-80 mesh, bottle of 10 g
Supelco
Carbopack Adsorbent, matrix Carbopack C, 60-80 mesh, bottle of 10 g
Supelco
Carbopack Adsorbent, matrix Carbopack C, 80-100 mesh, bottle of 10 g
Supelco
Carbopack Adsorbent, matrix Carbopack X, 40-60 mesh, bottle of 10 g
Supelco
Carbopack Adsorbent, matrix Carbopack X, 120-400 mesh, bottle of 50 g
Sigma-Aldrich
Zirconium, foil, thickness 0.1 mm, 99.98% trace metals basis
Sigma-Aldrich
Zirconium, rod, diam. 6.35 mm, ≥99% trace metals basis
Sigma-Aldrich
Zirconium, sponge, ≥99% trace metals basis
Supelco
Carbopack B, stainless steel TD tube, O.D. × L 1/4 × 3 1/2, unconditioned, pkg of 10 ea
Supelco
Carbopack B, glass TD tube, fritted, O.D. × L 1/4 in. × 3 1/2 in., preconditioned, pkg of 10 ea
Supelco
Carbopack B, glass TD tube, fritted, O.D. × L 1/4 in. × 3 1/2 in., unconditioned, pkg of 10 ea, matrix Carbopack
Supelco
FLM Carbopack X Deactivated Stainless Steel TD Tube, preconditioned, pkg of 10 tubes, O.D. × L 1/4 in. (6.35 mm) × 3 1/2 in. (89 mm)
Supelco
Carbopack B, O.D. × L 1/4 in. × 3 1/2 in., glass TD tube, fritted, Sealed with Brass Endcaps, preconditioned, pkg of 10 ea
Sigma-Aldrich
Olive oil, highly refined, low acidity
Supelco
Carbopack Adsorbent, matrix Carbopack B, 60-80 mesh, bottle of 10 g
Supelco
Olive oil, analytical standard
Sigma-Aldrich
Zirconium(IV) oxide, nanopowder, <100 nm particle size (TEM)
Sigma-Aldrich
Olive oil, tested according to Ph. Eur.
Sigma-Aldrich
Acetonitrile, anhydrous, 99.8%
Sigma-Aldrich
Zirconium(IV) oxide, powder, 5 μm, 99% trace metals basis
Sigma-Aldrich
Zirconium(IV) oxide, 99.99% trace metals basis (purity excludes ~2% HfO2)
Supelco
Acetonitrile, analytical standard
Sigma-Aldrich
Acetonitrile, electronic grade, 99.999% trace metals basis
Supelco
Supel QuE, Z-Sep/C18 Tube, centrifuge tube volume 2 mL, pack of 100
Supelco
Carbopack X, glass TD tube, fritted, O.D. × L 1/4 in. × 3 1/2 in., preconditioned, pkg of 10 ea
Supelco
Supel QuE, Z-Sep+ Bulk, pkg of 20 g
Sigma-Aldrich
Zirconium(IV) oxide, nanoparticles, dispersion, <100 nm particle size (BET), 10 wt. % in H2O
Sigma-Aldrich
Zirconium(IV) oxide, nanoparticles, dispersion, <100 nm particle size (BET), 5 wt. % in H2O
Supelco
Supel QuE, Z-Sep Tube, centrifuge tube volume 2 mL, pack of 100 ea