LC-MS/MS-Based Determination and Optimization of Linoleic Acid Oxides in <i>Baijiu</i> and Their Variation with Storage Time
<b>Background</b>: Post-production storage plays a pivotal role in developing the characteristic flavor profile of <i>Baijiu</i>, a traditional alcoholic beverage in China. While aging markers remain crucial for quality authentication, the identification of reliable metabolic...
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| Main Authors: | , , , , , , |
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| Format: | Article |
| Language: | English |
| Published: |
MDPI AG
2025-04-01
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| Series: | Metabolites |
| Subjects: | |
| Online Access: | https://www.mdpi.com/2218-1989/15/4/246 |
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| Summary: | <b>Background</b>: Post-production storage plays a pivotal role in developing the characteristic flavor profile of <i>Baijiu</i>, a traditional alcoholic beverage in China. While aging markers remain crucial for quality authentication, the identification of reliable metabolic indicators for chronological determination requires further exploration. <b>Methods</b>: This study establishes a novel liquid chromatography-tandem mass spectrometry (LC-MS/MS) methodology for quantifying five linoleic acid-derived oxidative metabolites in <i>Baijiu</i>: 9,12,13-trihydroxy-10(E)-octadecenoic acid (9,12,13-TriHOME), 9,10-Dihydroxy-12-octadecenoic acid (9,10-DiHOME), 9-oxo-(10E,12Z)-octadecadienoic acid (9-OxoODE), 9-hydroxy-(10E,12Z)-octadecadienoic acid (9-HODE) and 13-hydroxyoctadeca-(9Z,11E)-octadecadienoic acid (13-HODE). <b>Results</b>: The optimized protocol demonstrated exceptional sensitivity with limits of detection at 0.4 ppb through membrane-filtered direct dilution. Calibration curves exhibited excellent linearity (R<sup>2</sup> > 0.9990) across 1.0–100.0 ppb ranges. Method validation revealed satisfactory recovery rates (87.25–119.44%) at three spiking levels (10/20/50 ppb) with precision below 6.96% RSD. Application to authentic samples showed distinct temporal accumulation patterns. Light-aroma <i>Baijiu</i> exhibited storage duration-dependent increases in all five oxides. Strong aroma variants demonstrated significant positive correlations for 9,12,13-TriHOME, 9,10-DiHOME, and 9-OxoODE with aging time. <b>Conclusions</b>: These findings systematically characterize linoleic acid oxidation products as potential aging markers, providing both methodological advancements and new insights into <i>Baijiu</i> aging mechanisms. |
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| ISSN: | 2218-1989 |