Abstract

Acrylamide (AA) is a food contaminant in thermally processed products that is object of tight control. A simple and easy-to-apply methodology for routine monitoring of AA levels in food products could allow producers to be players in the control of their own products. In this work, a simple methodology for AA quantification without derivatization was developed for biscuits, for which the benchmark levels recommended by EFSA are 350 µg/kg, and 150 µg/kg for biscuits for infants and young children. Headspace-solid phase microextraction (HS-SPME) was used in 120 mL screwed-cap vials with a carboxen/polydimetylsiloxane fiber, 4 g of biscuits, and 10 mL of water during 15 min at room temperature under stirring. The addition of 30 mL of propanol under stirring during 15 min at room temperature and 15 min at 60 °C was used to promote AA transfer to the headspace. The fiber exposure was 45 min. A gas chromatography-mass spectrometry analysis allowed to obtain an external calibration curve at m/z 71, with linearity R2 > 0.99 and precision RSD < 9%. The detection and quantification limits were 27.4 µg/kg and 91.5 µg/kg, respectively. The methodology was successfully used in biscuits with lower AA amount, where mitigation strategies (asparaginase or pectate) were applied.

Highlights

  • Acrylamide (AA) is a food contaminant that can be found in processed products as chips, fries, biscuits, bread, and coffee

  • The aim of this study was to develop a simple and reliable methodology to quantify AA using Headspace-solid phase microextraction (HS-solid-phase microextraction (SPME)) followed by gas chromatography coupled with quadruple mass spectrometry detection (GC-qMS) in ion extraction chromatography (IEC) mode (m/z 71 and 55)

  • We propose a simple methodology for AA quantification based on direct extraction followed by quantification by GC-qMS (HS-SPME/GC-qMS) that does not require a complex sample preparation step

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Summary

Introduction

Acrylamide (AA) is a food contaminant that can be found in processed products as chips, fries, biscuits, bread, and coffee. To contribute to monitor and regulate its levels in food matrices by producers and authorities [4,5], it is important to have a simple, accessible, and reliable methodology to monitor AA concentration in thermally processed foods. Liquid chromatography-tandem mass spectrometry (LC-MS/MS) is the reference method for AA determination in food [9,10,11,12,13,14,15]. This methodology has the advantage of not requiring AA derivatization, but an extensive clean-up methodology for sample defatting and deproteinization is necessary [9]. Due to the complexity of food matrices, which account for a large number of water-soluble compounds that affect chromatographic separation and interfere with detection method, LC requires isotope-labeled internal standards such as d3-acrylamide [16,17,18] and 13C-3-acrylamide [16]

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