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

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.

Green Extraction Techniques as Advanced Sample Preparation Approaches in Biological, Food, and Environmental Matrices: A Review

“…SPME has been widely used to study the volatile composition of several foods, including walnut oils [109], hongeo [110], melon [111], and dairy products [112]. Moreover, this technique has also been used to determine the composition of specific analytes, such as the x-ray induced markers 2-dodecylcyclobutanone and 2-tetradecylcyclobutanone in irradiated dairy products [113], the contaminants 1,4-dioxane and 1,2,3-trichloropropane [114], acrylamide [115], organophosphorus pesticides [116], phthalates [117], synthetic phenolic antioxidants [118], and xanthines [119]. MSPD has been reported in the literature for the extraction of flavonoids [120], polyphenols [121], mangiferin, and hyperoside in mango-processing waste [122], ergosterol in edible fungi [123], and pharmacologically active substances in microalgae [124].…”

Low-Density Solvent-Dispersive Liquid–Liquid Microextraction with Phase Separation by Solidification of the Aqueous Phase for Analysis of Acrylamide in Vegetable and Fruit Chips by Gas Chromatography–Mass Spectrometry

“…Gas chromatography (GC) is widely used for acrylamide analysis due to its simplicity, automation capabilities, rapid data analysis, and high precision. Detectors such as flame ionization (FID), nitrogen–phosphorus (NPD), electron capture (ECD), , and mass spectrometry (MS) − have been employed to quantify acrylamide in food. However, detecting acrylamide by GC–MS can lead to low sensitivity due to its low molecular weight and high polarity.…”

Determination of 2-Pentanol Enantiomers via Chiral GC-MS and Its Sensory Evaluation in Baijiu

“…After extraction of the chiral compounds, the volatile analytes are usually analyzed using GC-MS, which has the advantages of good reproducibility, high resolution and efficiency [ 11 ]. In addition to this, there are several methods such as solid-liquid extraction (SLE) and stir sorptive bar extraction (SBSE), and multidimensional gas chromatography coupled with a time-of-flight mass spectrometer (MDGC-TOF-MS) [ 12 ]. Different types of extraction and detection methods can be selected depending on the complexity of the sample and/or the concentration level of the analytes.…”