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This paper reports on the development of a highly selective method for the determination of parts-per-billion (μg/kg) levels of 3-chloro-1,2-propandiol (3-MCPD) in hydrolysed vegetable proteins (HVP) using gas chromatography/ion trap mass spectrometry operating in the tandem mass spectrometry (MS/MS) mode. Samples were extracted into 5M sodium chloride solution and partitioned into diethyl ether using Extrelut® 20 solid phase columns. Dried and concentrated extracts were derivatized with heptafluorobutyrylimidazole (HFBI) prior to determination by gas chromatography ion trap (GC/IT) MS/MS. Multiple reaction monitoring was used to monitor the parent/daughter ion transitions of the analytes and the stable isotope internal standard (3-chloro-1,2-propandiol-d7). Calibration was linear over the range 5.0–500 pg/μL with correlation coefficients of 0.999 routinely obtained. The results showed that the method was capable of detecting 3-MCPD below 5 μg/kg in HVP when analysed by GC/ITMS/MS.
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Hamlet et al. (1997) studied this question.
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