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A miniaturized microwave-assisted saponification and extraction method for MOH analysis
Albendea, Paula; Ferrara, Donatella; Purcaro, Giorgia
2025
 

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Keywords :
Mineral oil saturated hydrocarbons; Mineral oil aromatic hydrocarbons; Miniaturaized saponification; Biological samples; LC/GC-FID; LC/GCxGC-FID/MS
Abstract :
[en] Mineral oil hydrocarbons (MOH), a complex group of lipid contaminants, consist of thousands of compounds categorized into saturated hydrocarbons (MOSH) and aromatic hydrocarbons (MOAH). Their AMDE —absorption, metabolism, distribution, and elimination—varies depending on their molecular structure. Therefore, distinguishing between different subclasses of MOSH (e.g., linear, branched, or cyclic alkanes) and MOAH (e.g., compounds with 1–2 or ≥3 rings) is crucial, which is possible thanks to the use of GC×GC. Analysing MOH in biological samples requires an efficient sample preparation method capable of removing interfering substances and concentrating MOH to improve sensitivity. Traditional methods often rely on saponification using large sample quantities (1–5 g), which limits their use in specific contexts such as human biomonitoring. This study aims to optimize a miniaturized microwave-assisted saponification and extraction (MASE) method for evaluating MOH in limited adipose tissue samples. The optimized method scales down the process described in prior research, testing tissue samples ranging from 100 to 400 mg. Saponification was conducted using only 2.5 mL each of hexane and KOH solution, enabled by an advanced microwave system that accommodates varying vessel sizes and operates under overpressure (~35 bars) at 120 °C for 20 minutes. The miniaturized MASE method demonstrated performance comparable to the original, with MOH recovery rates in line with JRC guidance requirements. Literature: [1] EFSA, J. EFSA 21 (2023) 1–143. [2] M. Biedermann and K. Grob. Journal of Chromatography A 1255 (2012), 56–75. [3] P. Albendea and G. Purcaro. Food Chemistry 480 (2025), 143880. [4] S. Bratinova, P. Robouch, E. Hoekstra and S. Bratinova (2023)2nd ed. Luxembourg: Publications Office of the European Union.
Research Center/Unit :
Gembloux Agro Bio Tech
Disciplines :
Chemistry
Author, co-author :
Albendea, Paula  ;  Université de Liège - ULiège > Département GxABT > Chemistry for Sustainable Food and Environmental Systems (CSFES)
Ferrara, Donatella ;  Université de Liège - ULiège > Gembloux Agro-Bio Tech > Gembloux Agro-Bio Tech ; UNITO - University of Turin > Dipartimento di Scienza e Tecnologia del Farmaco
Purcaro, Giorgia  ;  Université de Liège - ULiège > Département GxABT > Chemistry for Sustainable Food and Environmental Systems (CSFES)
Language :
English
Title :
A miniaturized microwave-assisted saponification and extraction method for MOH analysis
Publication date :
June 2025
Event name :
3rd Advance in Separation Sciences workshop
Event place :
Gembloux, Belgium
Event date :
From 12 to 13 of June 2025
Audience :
International
Commentary :
Acknowledgment The authors thank Milestone, LECO, and Restek for their support. This work is supported by ACESSS (Academic Center of Excellence for Separation Science and Sensing).
Available on ORBi :
since 08 July 2025

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