Determination of methacrylic acid in food simulants by pyrolytic butylation-gas chromatography

• Determination of methacrylic acid in food simulants by gas chromatography.
• Application of on–line pyrolytic alkylation technique without any pyrolyzer.
• Migration of methacrylic acid from plastic cup samples.

An on-line pyrolytic butylation approach was proposed to determine methacrylic acid (MA) in food simulants by gas chromatography (GC) without an expensive pyrolyzer. MA in food simulants was converted into butyl methacrylate in the presence of tetrabutylammonium hydroxide (TBAH) without any pretreatment at 330 °C in the injection-port, contributing to high GC signal response. The derivatizing conditions for the proposed method were optimized, namely the injection-port temperature, type and amount of the organic alkaline used for derivatization. A series of standard solutions of MA in the range of 1.0–50 mg/kg were analyzed with correlation coefficient r ≥ 0.9975. The limits of detection (LODs) were less than 0.15 mg/kg for MA in four matrix simulants (distilled water, 3% w/v acetic acid, 10% v/v ethanol, and isooctane). Relative standard deviations (RSDs) for retention time, peak height and peak area were all less than 3.88%. The technique was successfully applied to the analysis of MA migrating from plastic cup samples, with recoveries of added MA in the range of 96.5–123.0%. Direct injection of the simulants into the GC system after migration tests, without any pretreatment step, makes the developed method of great value for rapid screening analysis of samples in bulks.