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Cyclohexanone/sulfonated polymer catalyst: a new simple derivatizing procedure for GC-MS determination of 2- and 3-monochloropropanediols
Assessment of contamination of foods with monochloropropanediols (MCPD)
and subsequent mitigation of their formation is an important current issue of a
global food security. Methods for the determination of 2- or 3-MCPD in foods
at low µg/kg levels require analyte derivatization prior to gas chromatographymass
spectrometry (GC-MS) determination. All existing methods suffer from
various drawbacks associated with current derivatization schemes. We have
developed a new derivatization scheme, which uses cyclohexanone as a derivatization
agent and a sulfonated polymer as a solid-phase acidic catalyst. This derivatization
uses a readily available derivatization reagent and does not require any
postderivatization workup. The respective 2-MCPD 1,3-dioxane and 3-MCPD
1,3-dioxolane derivatives are stable with storage, produce characteristic molecular
ions, and chromatograph well on nonpolar GC columns. This derivatization
procedure was applied to the analysis of free 2- and 3-MCPD, bound 2- or 3-
MCPD (in the form of fatty acid esters after acidic hydrolysis), and also to simultaneous
analysis of free and bound forms. The method was tested on soy sauce,
commercial palm oil, palm oil noodles from an instant soup, and olive oil, which
was spiked with bound 2- and/or 3-MCPD. The results obtained using derivatization
with cyclohexanone agreed with the data obtained using traditional heptafluorobutyryl
imidazole derivatization. Additionally, data for soy sauce and palm
oil matrices obtained through interlaboratory testing programs had z-scores
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