No abstract

Chlorinated paraffins (CPs) are an emerging and ubiquitous group of environmental pollutants associated with adverse effects on human health, including endocrine disruption and possible carcinogenicity. In this study, supercritical fluid chromatography (SFC) and ultrahigh-performance liquid chromatography (UHPLC) — both coupled with high-resolution mass spectrometry (HRMS) — methods for the analysis of short-, medium-, and long-chain CPs in fish oil-based dietary supplements were developed and validated at concentration levels of 0.6 and 3.0 µg/g lipid weight (lw). The recoveries were in the range of 80–96% and repeatabilities, expressed as relative standard deviations, were <19%. The limits of detection for the UHPLC–HRMS method (from 0.03 to 0.05 µg/g lw) were 5 to 10 times lower than those obtained by SFC–HRMS (from 0.13 to 0.50 µg/lw).

2- and 3-chloropropane-1,2-diol (2- and 3-MCPD) and their fatty acid esters (2- and 3-MCPDEs) together with glycidyl fatty acids esters (GEs) belong to a group of process-induced contaminants. They are formed in high temperature environments and most commonly occur in refined vegetable oils. Since 2021, maximum limits for GEs and 3-MCPDEs have been enforceable in the EU, and the requirement for adequate analytical methods is constantly increasing. The aim of this study was to develop an efficient method to enable a rapid determination of nine 3-MCPDEs and seven GEs in vegetable oils within a single run employing supercritical fluid chromatography coupled to high-resolution tandem mass spectrometry (SFC–HRMS/MS). Contrary to a routine gas chromatography mass spectrometry method aimed at determination of the total MCPD pool, the sample throughput when using SFC–HRMS/MS was greatly increased, as the “dilute-and shoot” approach did not require any hydrolysis and derivatization. Additionally, the pattern of natural MCPDEs was characterized. The performance characteristics of this new method met the criteria required by Commision Regulation 2019/2093 for all target analytes.