Get access

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



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.

Get access to the full text of this article