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Single‐laboratory validation of a method to quantify bound 2‐chloropropane‐1,3‐diol and 3‐chloropropane‐1,2‐diol in foodstuffs using acid catalysed transesterification, HFBI derivatisation and GC/MS detection
Author(s) -
Hamlet Colin G.,
Asuncion Lisa
Publication year - 2011
Publication title -
european journal of lipid science and technology
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.614
H-Index - 94
eISSN - 1438-9312
pISSN - 1438-7697
DOI - 10.1002/ejlt.201000492
Subject(s) - repeatability , chemistry , chromatography , transesterification , diol , organic chemistry , catalysis
A protocol for the measurement of bound 2‐chloropropane‐1,3‐diol (2‐CPD) and 3‐chloropropane‐1,2‐diol 3‐CPD) in foodstuffs using acid catalysed transesterification and GC/MS/MS has undergone single‐laboratory validation. Validation of the method included an assessment of recovery (bias) of 3‐CPD from reference 3‐CPD mono‐ and diesters using a range of fortified and unfortified cereal, oil and potato products and participation in a EC proficiency test on 3‐CPD‐esters. Method repeatability was assessed by measuring bound 2‐ and 3‐CPD present in a processed cereal product. The results indicated that the method was fit for purpose for the measurement of bound 2‐ and 3‐CPD over concentration ranges of 40–10 000 µg/kg for oils, and 4–4000 µg/kg for foodstuffs depending on the fat content. The selectivity/robustness of the method was demonstrated by fortifying samples with ‘free’ 3‐CPD, chloride ions, glycerol and glycidyl butyrate: the procedure was found to be selective for ‘bound’ 3‐CPD and no adventitious formation of 2‐ or 3‐CPD occurred during analysis. Practical applications: This method provides a single‐laboratory validation of a method to measure amounts of bound 2‐ and 3‐CPD in a wide range food. The method provides the information necessary to assist researchers engaged in the selection and validation of analytical methods to measure these contaminants in foods.