HPLC-FLD simultaneous determination of 13 polycyclic aromatic hydrocarbons: validation of an analytical procedure for soybean oils

Abstract

Um método usando cromatografia líquida de alta eficiência com detecção por fluorescência (HPLC-FLD) foi desenvolvido para a determinação simultânea de 13 hidrocarbonetos policíclicos aromáticos (HPAs) em óleos de soja. A preparação das amostras envolve etapas de extração líquido-líquido com dimetilformamida-água (9:1 v/v), seguida de extração e pré-concentração dos HPAs em fase sólida utilizando cartuchos C-18. O método apresentou bons níveis de recuperação para a maioria dos HPAs estudados com valores entre 71 e 115%. As curvas de calibração obtidas se mostraram lineares dentro das respectivas faixas de trabalho (R 2 > 0,999). Os limites de detecção (LOD) e quantificação (LOQ) variaram entre 0,02-0,76 µg kg -1 e 0,03-0,96 µg kg -1 , respectivamente. O método foi aplicado para avaliar a contaminação dos óleos de soja comerciais mais consumidos no mercado brasileiro. A presença de HPAs foi confirmada em todas as amostras analisadas com valores médios na faixa de 0,20 a 5,93 µg kg -1 .A method using high performance liquid chromatography with fluorescence detection (HPLC-FLD) was developed for the simultaneous determination of 13 polycyclic aromatic hydrocarbons (PAHs) in soybean oils. The sample preparation includes liquid-liquid extraction with dimethylformamide-water (9:1, v/v) followed by a clean-up and concentration step with C-18 SPE cartridges. The method showed good recoveries for most of the PAHs studied with values between 71 and 115%. The calibration curves were linear over the range tested (R 2 > 0.999). Detection and quantification limits varied between 0.02-0.76 µg kg -1 and 0.03-0.96 µg kg -1 , respectively. The analytical procedure was successfully applied to evaluate the contamination of most consumed brands of soybean oils commercially available in the Brazilian market. The presence of PAHs was confirmed in all samples analyzed with mean values ranging from 0.20 to 5.93 µg kg -1 .Keywords: polycyclic aromatic hydrocarbons (PAHs), soybean oils, HPLC-fluorescence, organic contaminants, food analysis IntroductionThe occurrence of polycyclic aromatic hydrocarbons (PAHs) in food has attracted so much attention in the last few years because it is directly related to food safety. PAHs represent an important class of chemical carcinogens formed during incomplete combustion of organic material. Food is a significant source of PAHs for which human are exposed and their presence originate predominately from environmental pollution, during food processing (drying and smoking) and cooking (grilling, roasting, frying etc Camargo et al. 1355 Vol. 22, No. 7, 2011 the exception of benzo [ghi]perylene, have also shown clear carcinogenic effects in various types of bioassays in experimental animals. 13 During the JECFA sixty fourth meeting in 2005, the IPCS assessments and SCF re-evaluation of 33 compounds pointed the conclusion that 13 PAHs were clearly carcinogenic and genotoxic (Figure 1). 1 Except for benzo [ghi]perylene and cyclopenta [cd]pyrene, the compounds were the same as those stated by SCF. 1,13 Stu...

Adulteration and Presence of Polycyclic Aromatic Hydrocarbons in Extra Virgin Olive Oil Sold on the Brazilian Market

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Evaluation of polycyclic aromatic hydrocarbons content in different stages of soybean oils processing

“…The analytical procedure was based on previous one related to PAHs analysis in oils (Camargo et al, 2011a), however some modifications were introduced and the method was re-validated.…”

A stable mesoporous metal‐organic framework as highly efficient sorbent of dispersive micro solid‐phase extraction for the determination of polycyclic aromatic hydrocarbons by HPLC

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