Determination of Acrylamide in Foods by Liquid Chromatography–Tandem Mass Spectrometry with a Porous Graphitic Carbon Column

A high-performance liquid chromatography–tandem mass spectrometry (HPLC–MS/MS) method was established for the determination of acrylamide in foods using a porous graphitic carbon (PGC) column for separation. Samples were spiked with an isotopically labeled internal standard, extracted with acetonitrile–water, purified using a mixed-mode cation-exchange (MCX) solid-phase extraction cartridge, and then separated on a PGC column. By employing a single-step pass-through MCX clean-up, the inherent anti-interference capacity of the PGC column in complex matrices was evaluated. Methanol and 0.1% formic acid in water served as the mobile phase, and detection was performed in positive electrospray ionization mode with multiple reaction monitoring (MRM). Method validation was conducted using meat products and coffee samples, and the method was further applied to eight sample categories (n = 68), including potato chips, biscuits, instant coffee, and local specialty foods from southern Fujian. Acrylamide exhibited good linearity over the concentration range of 10–500 µg/L, with correlation coefficients of 0.9994–0.9998. The limit of detection (LOD) was 0.81–1.38 µg/kg, and the limit of quantification (LOQ) was 2.70–4.61 µg/kg. The mean spiked recovery was 94.2–103.4%, with a relative standard deviation (RSD) of 0.8–5.4%, and the matrix effect was 60.6–76.5% for the PGC column, compared with 46.8–51.3% for the C18 column. A paired t-test showed that the PGC column exhibited a significantly higher matrix effect (ME) value (i.e., less signal suppression) than the C18 column (p < 0.05). Owing to the strong retention characteristics of the PGC column for polar compounds, the method effectively improves chromatographic separation and reduces co-eluting interferences. It provides a practical approach for reducing matrix interference and improving sensitivity in matrices where interferences are well-controlled (e.g., meat products), while effectively overcoming the overestimation of acrylamide in highly complex matrices like coffee, with a residual matrix effect corrected by the isotope-labeled internal standard specifically within these validated matrices.