Analysis of Polynuclear Aromatic Hydrocarbons in Olive Oil after Solid-Phase Extraction Using a Dual-Layer Sorbent Cartridge Followed by High-Performance Liquid Chromatography with Fluorescence Detection

Abstract

A simple and easy direct solid-phase extraction (SPE) method was developed for the analysis of polynuclear aromatic hydrocarbons (PAHs) in olive oil using a dual-layer cartridge containing activated Florisil and a mixture of octadecyl (C18)-bonded and zirconia-coated silicas. Undiluted olive oil was applied directly to the SPE cartridge, and the sample was eluted with acetonitrile solvent. Background in the extract was found to be low enough for either gas chromatography-mass spectrometry (GC-MS) or high-performance liquid chromatography with fluorescence detection (HPLC-FLD) analysis. Average recoveries for 16 different PAHs from spiked olive oil replicates were >75%, with intraday precisions of <20% relative standard deviation (% RSD). Detection limits ranged from 0.2 to 1.0 μg/kg and, specifically for the PAHs listed in EC Regulation 835/2011, benzo(a)anthracene, chrysene, benzo(b)fluoranthene, and benzo(a)pyrene, were from 0.3 to 0.7 μg/kg. The method was then applied to determine the PAH content present in commercial samples of refined versus extra-virgin olive oils.

Study on the effect of activated carbon with bleaching earth on the reduction of polycyclic aromatic hydrocarbons (PAHs) in bleached soybean oil

“…The presence of these impurities in the oil causes darkness, foaming, reduction in smoke point and oxidative stability along with other adverse effects during the process, all of which eventually reduce the safety and quality of the finished product. Therefore, crude oil is supplied as an edible product subjected to processing and the removal of impurities (Yu et al, 2014;Stenerson et al, 2015). Polycyclic aromatic hydrocarbons (PAHs) are among the most toxic compounds in edible oils.…”

“…These compounds are also semi-volatile or non-volatile, non-degradable, highly organic, stable and toxic for the environment. (Stenerson et al, 2015;Singh et al, 2016).…”

“…The sample preparation includes liquid-liquid extraction with C18 SPE cartridges and analysis by the HPLC-FLD. (Camargo et al, 2011;Camargo et al, 2012;Stenerson et al, 2015;Akdogan et al, 2016;Dassilva et al, 2017). In addition, methods such as low temperature clean-up and solid-phase extraction (SPE) (Drabova et al, 2013;Payanan et al, 2013), and modified low-temperature and ultrasound-assisted liquid-liquid extraction method followed by HPLC/ FLD have been used for determining the levels of PAHs (Taghvaee et al, 2015a(Taghvaee et al, ,b, 2016.…”

Novel Uniform Fe3O4 Hollow Spheres for Magnetic Solid-phase Extraction of Polycyclic Aromatic Hydrocarbons

“…[6][7][8][9][10] Due to their trace amounts together with the complexity of the matrices, a sample preparation method is generally required before instrumental analysis. Solid-phase extraction (SPE) is one of the established and popular methods for sample enrichment due to its high extraction efficiency.…”

Dual‐layer solid‐phase extraction based on molecular imprinting technology: Seeking a route to enhance selectivity for trace analysis of pesticide residues in olive oil

“…As far as we are aware, the sample preparation approach explored in this work constitutes the first attempt on the development of a dual pesticide residue analysis based on SPE sorbents produced by molecular imprinting technology. Instead, other strategies described in the literature aiming to develop a multiresidue approach have explored the usefulness of a dual‐layer solid‐phase cartridge encompassing common SPE sorbents , but lead to a lack of selectivity and moreover none of them deals with the extraction/preconcentration of pesticide residues in olive oil matrices. Recently, a mixed‐bed SPE for atrazine herbicide from environmental water samples using MIP has been investigated ; nevertheless, this study encompasses the development of a SPE cartridge containing layers of an MIP selective for atrazine and silica not enabling a dual pesticide residue analysis, as attempted in the present study.…”