Determination of Light–Medium–Heavy Polycyclic Aromatic Hydrocarbons in Vegetable Oils by Solid-Phase Extraction and High-Performance Liquid Chromatography with Diode Array and Fluorescence Detection

Abstract

A new method for determination of 16 polycyclic aromatic hydrocarbons (PAHs)-naphthalene, acenaphthylene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benz[a]anthracene, chrysene, benzo[b]fluoranthene, benzo[k]fluoranthene, benzo[a]pyrene, dibenz[a,h]anthracene, benzo[g,h,i]perylene, and indeno[1,2,3-cd]pyrene-in vegetable oils was developed. Solid-phase extraction (SPE) prior to high-performance liquid chromatography with fluorescence detection could be used for all those PAHs except acenaphthylene. Acenaphthylene could be detected using a diode array detector at 228 nm. The parameters and variables that affect the extraction were investigated. Under optimum conditions: the extract reagent was centrifuged at 4 °C and evaporated. After that a SPE procedure was used for further cleanup. The limits of detection and limits of quantification were in the range of 0.01-2.35 and 0.04-7.00 μg kg(-1) in vegetable oil, respectively. The relative standard deviations were under 5%.

Polycyclic aromatic hydrocarbons in edible oils: An overview on sample preparation, determination strategies, and relative abundance of prevalent compounds

“…The optimum separation conditions usually imply a solvent gradient with ACN and water. Gradients normally start with a 40% to 50% ACN, in most cases (Barranco et al, 2003;Costopoulou et al, 2010;Gharbi et al, 2017;Martinez-López et al, 2005;Payanan et al, 2013;Shi et al, 2015Shi et al, , 2018Stenerson et al, 2015;Taghvaee et al, 2016;Teixeira et al, 2007;Yousefi et al, 2018;Zhao et al, 2013); then this concentration is linearly risen to 89% to 100% in an approximate time of 45 min, as so suggests ISO 15753:2016. Some reports have indicated the use of gradients with a higher proportion of ACN (70% to 85%) at the beginning of the run (Alves da Silva et al, 2017;Camargo et al, 2011;Ergönül & Sánchez, 2013;Ji et al, 2017;Molle et al, 2017;Moreda et al, 2004;Purcaro et al, 2008;Rodríguez-Acuña et al, 2008a;Tfouni et al, 2014).…”

“…As far as the flow rate is concerned, ISO 15753:2016 recommends a value of 1.2 mL/min. Some adjustments have been made with respect to this guidance, and flow has been also set at values of 1 mL/min (Barranco et al, 2003;Camargo et al, 2011;Costopoulou et al, 2010;Ergönül & Sánchez, 2013;Gharbi et al, 2017;Ji et al, 2017;Molle et al, 2017;Moreda et al, 2004;Rodríguez-Acuña et al, 2008a;Shi et al, 2018;Tfouni et al, 2014), 1.4 mL/min (Alarcón et al, 2012;Stenerson et al, 2015), and 1.5 mL/min (Dost & Ideli, 2012;Payanan et al, 2013;Purcaro et al, 2008;Teixeira et al, 2007;Wang, Lian, et al, 2018;Zhao et al, 2013). Alves da Silva et al (2017 focused on the determination of the set of PAH4 in some cold-pressed vegetable oils, applying a lower flow rate (0.4 mL/min) and a column with the following dimensions: 100 mm × 2.1 mm × 1.8 µm.…”

“…Another option to achieve Acy detection when pursuing the quantitative measurement of the complete set of EPA PAHs is the combination of the fluorimeter with a DAD detector. For example, Zhao et al (2013) have put into practice this alternative, determining this compound at 228 nm. The same occurs with the EU PAH CPP, which has to be determined by DAD at 222 nm (Costopoulou et al, 2010;Simon, Ruiz, Von Holst, Wenzl, & Anklam, 2008) or 254 nm (Ciecierska & Obiedziński, 2013).…”

Analytical approaches for measuring pesticides, mycotoxins and heavy metals in vegetable oils: A review

“…Many analytical methods employing cleanup procedures and chromatography methods have been reported for the determination of micro‐constituents and residues in lipid matrices, such as phenolic compounds, phytosterols, carotenoids, chlorophylls, 3‐monochloropropane‐1,2‐diol (3‐MCPD) and its esters, and polycyclic aromatic hydrocarbons (PAHs) . In 2009, a relatively recent review described the sample treatment methodologies for pesticide residue analysis in fatty vegetable matrices, including oilseeds and vegetable oils .…”

Cyclodextrin-promoted energy transfer for broadly applicable small-molecule detection

“…Such toxicants are potentially significant contributors to human disease (1–3), and are found in food supplies (4–6), water supplies (7) and in commercial products (8). Current methods for the detection of these chemical toxicants generally require multiple steps: (a) extraction of the toxicants from the environment (9); (b) purification of the toxicants via high-performance liquid chromatography (10) or gas chromatography (11) and (c) detection of the toxicants by mass spectrometry (12) or fluorescence spectroscopy (13). Such detection methods are limited in their ability to distinguish toxicants with identical molecular weights or similar fluorescence spectra.…”