A novel method for the simultaneous determination of esterified 2-/3-MCPD and glycidol in foods by GC-MS/MS

Several critical improvements for simultaneous determination of 2- and 3-monochlompropanediol esters (2-MCPDE, 3-MCPDE) and glycidyl esters (GE) were established in this study. GE were converted into 3-monobromopropanediol monoesters (3-MBPDE) through bromination, then, 3-MBPDE, 2-MCPDE and 3-MCPDE were converted into their free forms through acid catalysis. The three target analytes were purified by matrix solid phase dispersion extraction and then derivatized with heptafluorobutyrylimidazole (HFBI). The derivatives were detected by GC-MS/MS, and key parameters including NaBr concentration, bromination time and temperature, and transesterification time were optimized. Finally the new procedure was fully validated. The limits of detection for 3-MCPDE, 2-MCPDE and GE in vegetable oil were 2.0, 5.0, and 10 mu g/kg, respectively. The average recoveries ranged from 85.4% to 110% with relative standard deviation ( RSD ) of 1.3%-7.4% when the spiked levels varied from 0.05 to 1.0 mg/kg. The trueness of the method was also successfully and consistently evaluated by the proficiency test in FAPAS.

Automated summary

This study established critical improvements for simultaneous determination of 2-MCPDE, 3-MCPDE, and GE, with optimized parameters and validated results in vegetable oil samples. The method showed good detection limits, recoveries, and accuracy, as evaluated through proficiency testing.