A Novel Method for Simultaneous Monitoring of 2‐MCPD, 3‐MCPD and Glycidyl Esters in Oils and Fats

Abstract

The availability of a reliable methodology for the quantification of fatty acid esters of monochloropropropanediol (MCPD) and glycidol is essential for understanding the mechanism of formation of these process contaminants and for developing effective mitigation strategies. While several analytical methods for the determination of MCPD esters have already been developed and evaluated, only very few procedures are currently available for the analysis of glycidyl esters. This work presents a new indirect method for the simultaneous quantification of fatty acid esters of 2‐MCPD, 3‐MCPD and glycidol. The method is based on the acid‐catalyzed conversion of glycidyl esters into 3‐monobromopropanediol (3‐MBPD) monoesters which, owing to the structural similarity to MCPD esters, are quantified by using the procedure we previously optimized for the analysis of MCPD esters. The critical step of the method, which is the conversion of glycidyl esters, was optimized by testing different reagent concentrations and varying other condition settings. The novel method showed good repeatability (RSD <2.5 %) and between‐day reproducibility (RSD ≤5 %). The limit of detection was 0.04 mg/kg for bound 2‐MCPD and 3‐MCPD and 0.06 mg/kg for bound glycidol. The trueness of the method was evaluated by the analysis of spiked samples and by interlaboratory comparison.

Chloropropanols, Chloropropandiols and Their Esters in Food – Formation, Occurrence, Determination, Reduction of Content

“…Wyniki przeprowadzonych badań umoż-liwiły stwierdzenie, że rekomendowany zwykle 16-godzinny czas inkubacji próbek podczas transestryfikacji kwasowej może być skrócony do 4 h, bez istotnego wpływu na dokładność i powtarzalność wyników oznaczeń związanego 3-MCPD. Przeprowadzone badania pozwoliły autorom [22] na optymalizację i walidację metody jednoczesnego oznaczania estrów 2-MCPD, 3-MCPD i glicydolu. Oznaczenia wymienionych trzech analitów w wielu różniących się składem i pochodzeniem próbkach wykazały dużą dokładność, powtarzalność, czułość i wydajność opracowanej metody.…”

Occurrence of 3-MCPD and glycidyl esters in edible oils in the United States

“…This raised questions about the reliability of the hydrolysis techniques used in indirect methodology. The quality of indirect methodology has improved, and there are now several methods that appear to provide accurate quantitative information for these classes of contaminants (Kuhlmann 2011;Ermacora & Hrncirik 2013). As a response to the lack of reliability of the early indirect methods, direct approaches were developed for GEs (Blumhorst et al 2011;DuBois et al 2011;Firestone 2011;Haines et al 2011;Becalski et al 2012;Hori, Koriyama, et al 2012) and 3-MCPD esters (Haines et al 2011;Dubois et al 2012;Hori, Koriyama, et al 2012;Hori, Matsubara, et al 2012;Moravcova et al 2012;Yamazaki et al 2013) that do not require hydrolysis and analyse the fatty acid esters as they occur in processed oils without any structural modification.…”

Development of an analytical method for the simultaneous analysis of MCPD esters and glycidyl esters in oil-based foodstuffs

“…The oil sample obtained by the application of the procedure described in the previous section (fat extraction and purification) was dissolved in 2 ml of anhydrous tetrahydrofuran and treated according to a previously published method (Ermacora & Hrncirik 2013), recently adopted as AOCS Official Method (AOCS Cd 29a-13). In brief, 30 µl of acid aqueous solution of NaBr (3 mg ml −1 , H 2 SO 4 5%, v/v) were added to the sample, homogenised and the mixture was incubated at 50ºC for 15 min.…”