Development of an accurate and sensitive gas chromatographic method for the determination of acrolein content in Calvados and cider

Acrolein can be at the origin of an important organoleptic defect in beverages made from apples. Its content was investigated in freshly distilled Calvados and cider. The specificity of 3-methylbenzothiazolone hydrazine (MBTH) towards carbonyl compounds was used in order to derive acrolein in azines. Azines were separated and detected by gas chromatography coupled with a nitrogen-phosphorus Detector. Results showed that acrolein concentrations could be quickly determined in either Calvados or cider. Accuracy of quantification was better than 6% for concentrations about 1 mg/l in freshly distilled Calvados and 10% for concentrations about 10 μg/l in ciders. Acrolein content was found between 0.7 and 5.2 mg/l in samples of freshly distilled Calvados whereas it was between 7 and 15 μg/l in samples of cider. This method of quantification was applied to study disappearance kinetics of acrolein in cider. Acrolein content was found to decrease rapidly during the first hours and to change very slowly after a few days. Its behaviour during a distillation was also investigated showing that in spite of its high volatility it could also be found in the last fractions of distillation.