Novel approaches to analysis of 3-chloropropane-1,2-diol esters in vegetable oils

• Published in: Analytical and bioanalytical chemistry 2012-03, Vol.402 (9), p.2871-2883
• Main Authors: Moravcova, Eliska, Vaclavik, Lukas, Lacina, Ondrej, Hrbek, Vojtech, Riddellova, Katerina, Hajslova, Jana
• Format: Article
• Language: English
• Subjects: alpha-Chlorohydrin; Analysis; Analytical Chemistry; Biochemistry; Characterization and Evaluation of Materials; Chemistry; Chemistry and Materials Science; Chromatography, High Pressure Liquid - methods; Contaminants; Diesters; Esters; Esters - analysis; Food Science; Glycerol - analogs & derivatives; Glycerol - analysis; Glycols (Class of compounds); Helianthus; High performance liquid chromatography; Ionization; Laboratory Medicine; Liquid chromatography; Mass spectrometry; Mass Spectrometry - methods; Monitoring/Environmental Analysis; Original Paper; Plant Oils - analysis; Quantitative analysis; Sunflower oil; Vegetable oils
• ISSN: 1618-2642; 1618-2650
• DOI: 10.1007/s00216-012-5732-1

A sensitive and accurate method utilizing ultra-high 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 real-life 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.