HS-SPME Gas Chromatography Approach for Underivatized Acrylamide Determination in Biscuits


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 mu g/kg, and 150 mu g/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 degrees 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 R-2 > 0.99 and precision RSD < 9%. The detection and quantification limits were 27.4 mu g/kg and 91.5 mu g/kg, respectively. The methodology was successfully used in biscuits with lower AA amount, where mitigation strategies (asparaginase or pectate) were applied.



subject category

Food Science & Technology


Passos, CP; Petronilho, S; Serodio, AF; Neto, ACM; Torres, D; Rudnitskaya, A; Nunes, C; Kukurova, K; Ciesarova, Z; Rocha, SM; Coimbra, MA

our authors


This work received financial support from PT national funds (FCT/MCTES, Portuguese national funding agency for science, research and technology) for the financial support to LAQV-REQUIMTE (UIDB/50006/2020), CESAM (UIDB/50017/2020; UIDP/50017/2020), and CICECO (UIDB/50011/2020 & UIDP/50011/2020) Research Units through national founds and, where applicable, co-financed by the FEDER, within the PT2020 Partnership Agreement, and Compete 2020. This publication was also supported by the Operational program Integrated Infrastructure within the project: Demand-driven research for the sustainable and innovative foods, Drive4SIFood, 313011V336, cofinanced by the European Regional Development Fund. Claudia Passos contract (CEECIND/01873/2017) and Silvia Petronilho post-doc grant (SFRH/BPD/117213/2016) was supported by FCT.

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