Comparative analysis of ultrasound-accelerated alkaline and acid hydrolysis for the indirect determination of 3-monochloropropane-1,2-diol fatty acid esters

• Published in: Journal of food composition and analysis Vol. 125; p. 105764
• Main Authors: Custodio-Mendoza, Jorge A., Arribas García, Alberto, Lorenzo Ferreira, Rosa A., Carro Díaz, Antonia M.
• Format: Journal Article
• Language: English
• Published: Elsevier Inc 01.01.2024
• Subjects: 3-MCPD; Edible oils; Fatty acid esters; GC–MS; Indirect method; Ultrasound-assisted; AOCS; 3-MCPD; FDA; RSD; GC–MS; HFBI; 3-MCPDE; Fatty acid esters; IARC; PBA; EFSA; QC; Indirect method; Ultrasound-assisted; BSTFA; 3-MCPDd5; Edible oils; DLLME; EVO
• ISSN: 0889-1575; 1096-0481
• DOI: 10.1016/j.jfca.2023.105764

Ultrasound-accelerated hydrolysis is effectively used for the first time in the release of 3-monochloropropane-1,2-diol (3-MCPD) from its fatty esters. Indirect determination of 3-MCPDE fatty acid esters was performed under alkaline and acid conditions using sodium methoxide and sulfuric acid, respectively, prior to GC-MS analysis. Dispersive liquid-liquid microextraction (DLLME) was used to derivatize the free 3-MCPD with n-heptafluorobutyrylimidazole (HFBI). Two asymmetrical screening designs were used to evaluate parameters affecting the methods’ performances: time, temperature, hydrolytic agent volume, and concentration. A comparative study between both methods was performed. Research showed that comparable results are achieved in terms of linearity (r2 > 0.9995), specificity, accuracy, and precision. Determination limits were lower for the alkaline method (67 ng g−1). Twenty samples of four types of edible oil were assessed using both methods: extra virgin olive oil (EVO), refined sunflower oil, refined olive oil, and palm oil. Results obtained here were comparable and similar to those reported in the literature. Alkaline hydrolysis was the recommended approach and should be used in occurrence studies. •Two novel indirect approaches for 3-MCPD were developed and validated.•Acid and basic hydrolysis of 3-MCPD esters were ultrasound-accelerated.•HFBI derivatization is performed during DLLME prior GC-MS analysis.•20 edible oil samples were analyzed for 3-MCPD presence.•Alkaline approach reduced consumption of reagents and time.