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Updated: Jun 25, 2026
Single-throughput Complementary High-resolution Analytical Techniques for Characterizing Complex Natural Organic Matter Mixtures
Published on: January 7, 2019
A sensitive UHPLC-QqQ-MS/MS method for the simultaneous analysis of MDA/4-HHE/4-HNE in edible oils and nuts was
Jiajun Chen1, Nan Zhu2, Feixuan Wang2
1Nanjing Institute of Product Quality Inspection (Nanjing Institute of Quality Development and Advanced Technology Application), Nanjing 210019, China; School of Life Sciences, Nanjing University, Nanjing 210023, China.
Abstract:
A novel and sensitive method using ultra-high performance liquid chromatography-tandem triple quadrupole mass spectrometry (UHPLC-QqQ-MS/MS) was developed for the simultaneous determination of three lipid oxidation markers: malondialdehyde (MDA), 4-hydroxy-2-hexenal (4-HHE) and 4-hydroxy-2-nonenal (4-HNE) in edible oils and nuts. Optimization of 2,4-dinitrophenylhydrazine (DNPH) derivatization and solid-phase extraction (SPE), combined with isotope compensation to ensure high analytical performance: linearity (R2 ≥ 0.9990), precision (RSD ≤ 18.75%), accuracy (SD ≤ 19.24%), recovery (80.34-119.78%). Limit of detection (LOD) and limit of quantification (LOQ) ranged from 0.25 μg/kg and 0.50-2.50 μg/kg, respectively. This validated method was further applied to monitor lipid peroxidation levels, revealed that thermal processing significantly increases MDA/4-HHE/4-HNE contents, which reached 7.80 mg/kg from 26.50 μg/kg in oils and 0.98 mg/kg from 8.27 μg/kg in nuts. Notably, the accumulation of MDA and 4-HHE in edible oils was approximately ten fold higher than in nuts.
