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Collaborative Study for the Quantification of Total Contents of 2- and 3-Monochloropropanediol and Glycidol in Food Emulsifiers by GC-MS
  • Jan Kuhlmann
Jan Kuhlmann
SGS Germany GmbH
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An international robin round was carried out to validate a method for the quantification of 2-monochloropropane-1,3-diol (2-MCPD), 3-monochloropropane-1,2-diol (3-MCPD) and 2,3-epoxy-1-propanol (Glycidol) being present as fatty acid esters in plant-based food emulsifiers. The evaluated method was a modification of the American Oil Chemist´s Society (AOCS) Official Method Cd29b-13. Briefly, this method consists from parallel analysis of two sample aliquots that are spiked with different sets of internal standards. Mild alkaline interesterification overnight in the freezer releases the core analytes. Reaction stop and glycidol conversion into monobromopropanediol (MBPD) is realised by addition of acidified sodium bromide solution. Subsequently, matrix removal and analyte extraction are achieved by two liquid/liquid (l/l) extraction steps. After derivatisation with phenylboronic acid (PBA) the final extracts are analysed by gas chromatography-mass spectrometry (GC-MS). Quantification is carried out by internal one-point-calibration. 6 laboratories from 4 European countries participated in the trial and reported 8 data sets for 10 test materials (mono- and diacylglycerides as well as polyglycerol polyricinoleates) that were analysed as blind duplicates, giving a total of 20 samples. Result outliers were eliminated according to accepted standards. At 2-MCPD levels above 0.02 mg/kg, 3-MCPD levels above 0.06 mg/kg and glycidol levels above 0.22 mg/kg repeatability (RSDr) ranged from 1.5 % to 24.9 %, reproducibility (RSDR) ranged from 7.8 % to 29.0 % and HORRATR-values ranged from 0.5 to 1.7. The tested method showed to be suitable for the determination of 2-MCPD, 3-MCPD and glycidol in food emulsifiers consisting from mono- and diacylglycerides as well as polyglycerol polyricinoleates.
16 Jun 2021Submitted to Journal of the American Oil Chemists' Society
16 Jun 2021Submission Checks Completed
16 Jun 2021Assigned to Editor
29 Jun 2021Reviewer(s) Assigned
23 Jul 2021Review(s) Completed, Editorial Evaluation Pending
27 Jul 2021Editorial Decision: Revise Minor
17 Aug 20211st Revision Received
17 Aug 2021Submission Checks Completed
17 Aug 2021Assigned to Editor
17 Aug 2021Reviewer(s) Assigned
08 Sep 2021Review(s) Completed, Editorial Evaluation Pending
16 Sep 2021Editorial Decision: Accept
11 Oct 2021Published in Journal of the American Oil Chemists' Society. 10.1002/aocs.12545