A method for determination of acrylamide in bread by UPLC-MS/MS

Acrylamide is a contaminant present especially in baked and fried rich starchy food products, such as french fries, bread, cookies and coffee. It is a product of the Maillard Reaction formed during food processing, at high temperatures by the reaction between free amine groups (amino acids/proteins) and the carbonyl group (sugars/carbohydrates). Acrylamide is classified by the International Agency for Research on Cancer as a carcinogenic substance to humans, and its quantification is essential to control the exposure risk. Since the discovery of its presence in food, several studies have been conducted to developed extraction procedures for acrylamide quantification. The present study aims to develop a cleaning method suitable for several food matrices, like bread and chips, followed by liquid chromatography coupled to a mass detector method (LC-MS/MS) for acrylamide quantification. To achieve this aim, the use of solid-phase extraction and several salts mixtures, such as QuEChERS type, was implemented. The results obtained through the application of mixture 1 (figure 1) were not satisfactory. In this case we observed the tailing effect as well as low recovery of the internal standard, with recovery values below 50%. For the extraction method using mixture 2 (figure 2 and 3) the results were satisfactory, where a spike recovery between 85 to 112% was obtained and the results of the certified reference material varied between 71 and 80 µg/kg, which is within the range of uncertainty. The acrylamide response was linear over a concentration range of 5 to 80 µg/L with a correlation coefficient of the calibration curve above 0.995. The limit of quantification (LOQ) was established at 5 mg/kg. The presented method, LC-MS/MS, with mixture 2 is adequate for the determination of acrylamide in bread , accomplishing the performance criteria of the regulation published by the European Commission, COMMISSION REGULATION (EU) 2017/2158 of 20 November 2017.

The authors appreciate the financial support of MISAGE project LISBOA-01-0145-FEDER-024172). This project has received financial support from the Fundação para a Ciência e a Tecnologia (FCT), Portugal.

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