Department of Analytical Chemistry, Faculty of Chemistry, Gdańsk University of Technology, 11/12 G. Narutowicza Street, 80-233, Gdańsk, Poland.
EcoTech Center, Gdańsk University of Technology, 11/12 G. Narutowicza Street, 80-233, Gdańsk, Poland.
Anal Bioanal Chem. 2024 Feb;416(5):1117-1126. doi: 10.1007/s00216-023-05107-6. Epub 2023 Dec 21.
For the analysis of plant-based meat substitutes and the determination of Maillard reaction products such as acrylamide, 5-hydroxymethylfurfural and furaneol, a novel and effective procedure based on hydrophobic natural deep eutectic solvent and liquid chromatography coupled with tandem mass spectrometry was developed for the first time. The 49 compositions of the deep eutectic solvents were designed and screened to select the most suitable option. The terpenoids eugenol and thymol in a molar ratio of 2:1 were selected as precursors for solvent formation, allowing effective extraction of the target analytes. The developed procedure comprised two main steps: extraction - in which the analytes are isolated from the solid sample due to the salting-out effect and pre-concentrated in the deep eutectic solvent, and back-extraction - in which the analytes are re-extracted into the formic acid solution for subsequent mass spectrometric detection. As the density of the aqueous phases changed during the extraction and back-extraction steps, the phenomenon of inversion of the coalesced organic phase was observed, which simplified the withdrawing of the phases. The linear range was 1-50 ng/mL for acrylamide, 10-1000 ng/mL for 5-hydroxymethylfurfural and 200-1000 ng/mL for furaneol with coefficients of determination above 0.9952. The developed method was fully validated and found recoveries were in the range 83-120%, with CVs not exceeding 4.9%. The method was applied to real sample analysis of pea-based meat substitutes.
首次开发了一种基于疏水性天然深共晶溶剂和液相色谱-串联质谱法的新型有效方法,用于分析植物性肉类替代品和测定美拉德反应产物,如丙烯酰胺、5-羟甲基糠醛和糠醇。设计和筛选了 49 种深共晶溶剂的组成,以选择最合适的方案。选择萜烯丁香酚和百里酚以 2:1 的摩尔比作为溶剂形成的前体,允许有效提取目标分析物。所开发的方法包括两个主要步骤:提取 - 由于盐析效应,将分析物从固体样品中分离出来,并在深共晶溶剂中预浓缩,以及反提取 - 将分析物重新提取到甲酸溶液中,以便进行后续的质谱检测。由于在提取和反提取步骤中水相的密度发生变化,观察到凝聚有机相的反转现象,这简化了相的抽取。丙烯酰胺的线性范围为 1-50ng/mL,5-羟甲基糠醛的线性范围为 10-1000ng/mL,糠醇的线性范围为 200-1000ng/mL,相关系数均大于 0.9952。该方法经过充分验证,发现回收率在 83-120%之间,CV 不超过 4.9%。该方法应用于豌豆基肉类替代品的实际样品分析。