article · Foods
A new testing method determines free glycidol and total free monochloropropanediol (MCPD) contaminants in fish and krill oil. The protocol relies on high-performance liquid chromatography-tandem mass spectrometry paired with p-(dimethylamino)phenol derivatisation. Sample preparation uses an aqueous sodium chloride extraction alongside C18 sorbent clean-up to break emulsions, separating glycidol and MCPD under weak acidic and strong alkaline conditions. The technique demonstrates broad linearity between 1 and 256 ng per millilitre, achieving a detection limit of 0.5 ng per millilitre and a quantification limit of 1 ng per millilitre, which offers higher sensitivity than standard gas chromatography-mass spectrometry methods. Testing on commercial dietary supplements confirmed MCPD in fish oil at levels up to 32.78 ng per millilitre, while krill oil samples contained MCPD up to 2767.3 ng per millilitre and glycidol up to 22.2 ng per millilitre.
Fish and krill oils are widely consumed dietary supplements, but processing can introduce potentially harmful contaminants such as free glycidol and monochloropropanediol. Providing an analytical technique with greater sensitivity and simpler preparation allows food safety authorities and manufacturers to monitor these chemical residues more accurately, ensuring marine oil supplements meet quality and safety benchmarks.
This method is an applied analytical protocol already tested on commercial dietary supplements. It offers food testing laboratories, supplement manufacturers, and quality assurance services a sensitive alternative to conventional gas chromatography procedures. The approach is near-market for analytical service providers and could also be adapted to detect esterified forms, supporting routine compliance screening across edible oil supply chains.
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This study introduces a novel method for detecting free glycidol and total free monochloropropanediol (MCPD) in fish and krill oil. Before analysis on high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS), <i>p</i>-(dimethylamino)phenol was used for derivatization of these compounds, enabling the sensitive determination of these contaminants. The sample preparation procedure includes a simple, efficient pretreatment using NaCl aqueous solution extraction and C18 sorbent cleanup (for demulsification), distinguishing glycidol from MCPD under varied reaction conditions for derivatization (weak acidic and strong alkaline aqueous environments). This approach shows broad linearity from 1 to at least 256 ng·mL<sup>-1</sup>, improved sensitivity compared to standard GC-MS methods, with the limit of detection (LOD) and limit of quantification (LOQ) for MCPD and glycidol in both oil samples verified at 0.5 ng·mL<sup>-1</sup> and 1 ng·mL<sup>-1</sup>, respectively. Different from previous HPLC-MS methods for direct detection of glycidol esters or MCPD esters, this is the first HPLC-MS method used for the detection of free glycidol and total free MCPD in edible oil. Furthermore, this method can be potentially developed for glycidol or monochloropropane diol esters, which is similar to the current official methods adopted for indirect detection of these contaminants in different food matrices. Application of this detection method to real dietary supplements (fish oil and krill oil) revealed MCPD residues in fish oil (maximum detected: 32.78 ng·mL<sup>-1</sup>) and both MCPD (maximum detected: 2767.3 ng·mL<sup>-1</sup>) and glycidol (maximum detected: 22.2 ng·mL<sup>-1</sup>) in krill oil, emphasizing its effectiveness and accuracy for assessing contamination in these supplements.
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DOI: 10.3390/foods13152340
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