Determination of Acrylamide in Foods by Liquid Chromatography–Tandem Mass Spectrometry with a Porous Graphitic Carbon Column
- 1Department of Physical and Chemical Laboratory, Quanzhou Center for Disease Control and Prevention (Quanzhou Health Supervision Institute), Quanzhou 362000, China
- 2The Affiliated Quanzhou Center for Disease Control and Prevention of Fujian Medical University, Quanzhou 362000, China
Abstract
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.
Related
- Ultra-High-Performance Liquid Chromatography-High Resolution Mass Spectrometry and Gas Chromatography-Mass Spectrometry Screening of Classical Psychoactive Substances, Novel Psychoactive Substances, and Metabolites in Postmortem Urine Samples
- Efficient dual-mode liquid chromatography–tandem mass spectrometry methods for quantifying major cyanotoxins in natural water
- The Development of a Simple Liquid Chromatography‐Precursor Ion Scan‐Mass Spectrometry Screening Method for the Detection of Phytocannabinoids in Plant Extracts
- Preliminary pharmacokinetic investigation of two discoidin domain receptor 2 inhibitors in murine plasma and brain using liquid chromatography–tandem mass spectrometry analysis
- Precision Profiling of α‐1,4‐ Versus α‐1,6‐Glycosidase Activity Through Synthetic Linear and Branched Glycogen Tetramers Using Cyclic Ion Mobility Mass Spectrometry and High‐Performance Liquid Chromatography‐Mass Spectrometry
BibTeX
@article{chen2026determination,
title = {{Determination of Acrylamide in Foods by Liquid Chromatography–Tandem Mass Spectrometry with a Porous Graphitic Carbon Column}},
author = {Huijiao Chen and Lingang Chen and Weiping Xie},
journal = {Molecules},
year = {2026},
month = nov,
doi = {10.3390/molecules31213981},
url = {https://www.mdpi.com/1420-3049/31/21/3981},
note = {CC BY 4.0},
}
RIS
TY - JOUR
TI - Determination of Acrylamide in Foods by Liquid Chromatography–Tandem Mass Spectrometry with a Porous Graphitic Carbon Column
AU - Huijiao Chen
AU - Lingang Chen
AU - Weiping Xie
PY - 2026
DA - 2026/11/04
JO - Molecules
DO - 10.3390/molecules31213981
UR - https://www.mdpi.com/1420-3049/31/21/3981
AB - 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.
SN - 1420-3049
ER -