1. Single-laboratory validation of a saponification method for the determination of four polycyclic aromatic hydrocarbons in edible oils by HPLC-fluorescence detection
- Author
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Thomas Wenzl, Abdullah Akdogan, and Gerhard Buttinger
- Subjects
Chrysene ,Aromatic compounds ,Chromatography, High Pressure Liquid ,Fluorescence ,Laboratories ,Plant Oils/*chemistry ,Polycyclic Aromatic Hydrocarbons/*analysis ,Solid Phase Extraction ,Spectrometry, Fluorescence ,Health, Toxicology and Mutagenesis ,limit of quantitation ,polycyclic aromatic hydrocarbons ,Aromatic hydrocarbons ,Extraction ,chrysene ,Toxicology ,01 natural sciences ,chemistry.chemical_compound ,Oils and fats ,Concentration levels ,Single laboratory validations ,Sample preparation ,Solid phase extraction ,Polycyclic Aromatic Hydrocarbons ,corn oil ,benzo[b]fluoranthene ,media_common ,Liquid partitioning ,Chromatography ,limit of detection ,Saponification ,Hydrolysis ,Pyrene ,benzo[a]pyrene ,liquid liquid extraction ,04 agricultural and veterinary sciences ,General Medicine ,olive oil ,040401 food science ,Method validations ,vegetable oil ,priority journal ,validation study ,Aromatization ,Uncertainty analysis ,sunflower oil ,fluorescence ,measurement accuracy ,high performance liquid chromatography ,benz[a]anthracene ,Liquid chromatography ,Phase separation ,chemistry ,Article ,0404 agricultural biotechnology ,polycyclic aromatic hydrocarbon ,media_common.cataloged_instance ,Plant Oils ,HPLC-fluorescence detection ,European union ,high-performance liquid chromatography ,sesame seed oil ,Fluoranthene ,Detection limit ,Solid-phase extraction ,010401 analytical chemistry ,Public Health, Environmental and Occupational Health ,Edible oil ,Limits of detection ,spectrofluorometry ,Liquids ,General Chemistry ,Hydrocarbons ,0104 chemical sciences ,Relative measurement ,measurement repeatability ,laboratory ,Food Science - Abstract
An analytical method is reported for the determination of four polycyclic aromatic hydrocarbons (benzo[a]pyrene (BaP), benz[a]anthracene (BaA), benzo[b]fluoranthene (BbF) and chrysene (CHR)) in edible oils (sesame, maize, sunflower and olive oil) by high-performance liquid chromatography. Sample preparation is based on three steps including saponification, liquid–liquid partitioning and, finally, clean-up by solid phase extraction on 2 g of silica. Guidance on single-laboratory validation of the proposed analysis method was taken from the second edition of the Eurachem guide on method validation. The lower level of the working range of the method was determined by the limits of quantification of the individual analytes, and the upper level was equal to 5.0 µg kg-1. The limits of detection and quantification of the four PAHs ranged from 0.06 to 0.12 µg kg-1 and from 0.13 to 0.24 µg kg-1. Recoveries of more than 84.8% were achieved for all four PAHs at two concentration levels (2.5 and 5.0 µg kg-1), and expanded relative measurement uncertainties were below 20%. The performance of the validated method was in all aspects compliant with provisions set in European Union legislation for the performance of analytical methods employed in the official control of food. The applicability of the method to routine samples was evaluated based on a limited number of commercial edible oil samples. © 2016 The Author(s). Published by Taylor & Francis.
- Published
- 2016