title: Novel approaches to analysis of 3-chloropropane-1,2-diol esters in vegetable oils.
abstract: A sensitive and accurate method utilizing ultrahigh performance liquid chromatography (U-HPLC) coupled to high resolution mass spectrometry based on orbitrap technology (orbitrapMS) for the analysis of nine 3-chloropropane-1,2-diol (3-MCPD) diesters in vegetable oils was developed. To remove the interfering triacylglycerols that induce strong matrix effects, a clean-up step on silica gel column was used. The quantitative analysis was performed with the use of deuterium-labeled internal standards. The lowest calibration levels estimated for the respective analytes ranged from 2 to 5 μg kg(-1). Good recovery values (89-120%) and repeatability (RSD 5-9%) was obtained at spiking levels of 2 and 10 mg kg(-1). As an alternative, a novel ambient desorption ionization technique, direct analysis in real time (DART), hyphenated with orbitrapMS, was employed for no separation, high-throughput, semi-quantitative screening of 3-MCPD diesters in samples obtained by chromatographic fractionation. Additionally, the levels of 3-MCPD diesters measured in reallife vegetable oil samples (palm oil, sunflower oil, rapeseed oil) using both methods are reported. Relatively good agreement of the data generated by U-HPLC-orbitrapMS and DART-orbitrapMS were observed. With regard to a low ionization yield achieved for 3-MCPD monoesters, the methods presented in this paper were not yet applicable for the analysis of these contaminants at the naturally occurring levels.
authors.affiliation: Department of Food Chemistry and Analysis, Institute of Chemical Technology, Prague, Czech Republic.
authors.forename: Eliska
authors.initials: E
authors.lastname: Moravcova
authors.forename: Lukas
authors.initials: L
authors.lastname: Vaclavik
authors.forename: Ondrej
authors.initials: O
authors.lastname: Lacina
authors.forename: Vojtech
authors.initials: V
authors.lastname: Hrbek
authors.forename: Katerina
authors.initials: K
authors.lastname: Riddellova
authors.forename: Jana
authors.initials: J
authors.lastname: Hajslova
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004952:Esters / Q000032:analysis*; D005990:Glycerol / Q000031:analogs & derivatives* / Q000032:analysis; D013058:Mass Spectrometry / Q000379:methods*; D010938:Plant Oils / Q000032:analysis*; D000517:alpha-Chlorohydrin
chemical_list: D004952:Esters; D010938:Plant Oils; D000517:alpha-Chlorohydrin; D005990:Glycerol