矿物油芳香烃的纯化及基于芳香烃环数的液相色谱柱分离。环氧化的替代品。

IF 3.8 2区 化学 Q1 BIOCHEMICAL RESEARCH METHODS Journal of Chromatography A Pub Date : 2025-01-15 DOI:10.1016/j.chroma.2025.465684
Aleksandra Gorska , Grégory Bauwens , Marco Beccaria , Giorgia Purcaro
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引用次数: 0

摘要

目前,植物油中矿物油芳烃(MOAH)的分析由于样品制备和数据解释等各种因素而具有很高的不确定性。一个重要的因素是在色谱分析中萜烯类生物源化合物与MOAH组分的共洗脱。常用的纯化方法是环氧化,这是一种改变干扰极性的化学反应,使其与MOAH分离。然而,这种反应是非选择性的,可能导致MOAH和内部标准的损失。当使用具有较高反应动力学的环氧化程序时,例如使用过甲酸的程序,这种变化尤其明显。MOAH损失也因其组成而异,这是不可预测的。此外,2-甲基萘(2MN)和1,3,5-三叔丁基苯(TBB)作为常用的定量标准,其损失速率也不同。因此,最终的MOAH数量将根据所使用的标准及其初始成分而变化。本工作提出了一种新的纯化方法,基于二氧化硅的液相色谱分离,使用与通常的MOSH/MOAH分离相同的柱和洗脱液。这种方法有效地去除角鲨烯、胡萝卜素及其衍生物,而不会像环氧化那样在内标和MOAH之间造成不一致的损失。不同MOAH来源和浓度的椰子油、棕榈油、葵花籽油和橄榄油中MOAH的平均回收率为94%(±8%)。此外,对单/二芳MOAH和其他多芳MOAH的单独分析和定量提出了展望。这是特别有趣的,因为这两个亚组分与不同的毒理学性质有关。
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Purification of mineral oil aromatic hydrocarbons and separation based on the number of aromatic rings using a liquid chromatography silica column. An alternative to epoxidation
The analysis of mineral oil aromatic hydrocarbons (MOAH) in vegetable oils is currently associated with high uncertainty due to various factors ranging from sample preparation to data interpretation. One significant factor is the coelution of biogenic compounds of terpenic origin with the MOAH fraction during chromatographic analysis. The common purification method is epoxidation, a chemical reaction that changes the polarity of the interferences, allowing their separation from MOAH. However, this reaction is non-selective and can lead to losses of both MOAH and internal standards. This variation is especially noticeable when using epoxidation procedures with higher reaction kinetics, such as those employing performic acid. MOAH losses also vary depending on their composition, which is unpredictable. Furthermore, 2-methylnaphthalene (2MN) and 1,3,5-tri‑tert-butylbenzene (TBB), which are the common quantification standards, are lost at different rates. As a consequence, the final MOAH quantity will vary both depending on the standard used, and on its initial composition. This work presents a new purification approach based on liquid chromatography fractionation on silica using the same column and eluents as for the usual MOSH/MOAH fractionation. This approach efficiently removes squalene, carotenes, and derivatives, without inducing inconsistent losses between the internal standards and MOAH as epoxidation does. On average, MOAH recovery using this new method was 94% (± 8%) in coconut, palm, sunflower, and olive oil, using different MOAH sources and concentrations. Additionally, perspectives are presented regarding the separate analysis and quantification of mono-/diaromatic MOAH and other polyaromatic MOAH. This is of particular interest as these two sub-fractions are associated with different toxicological properties.
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来源期刊
Journal of Chromatography A
Journal of Chromatography A 化学-分析化学
CiteScore
7.90
自引率
14.60%
发文量
742
审稿时长
45 days
期刊介绍: The Journal of Chromatography A provides a forum for the publication of original research and critical reviews on all aspects of fundamental and applied separation science. The scope of the journal includes chromatography and related techniques, electromigration techniques (e.g. electrophoresis, electrochromatography), hyphenated and other multi-dimensional techniques, sample preparation, and detection methods such as mass spectrometry. Contributions consist mainly of research papers dealing with the theory of separation methods, instrumental developments and analytical and preparative applications of general interest.
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