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Development and validation of LC-MS-based alternative methodologies to GC-MS for the simultaneous determination of triterpenic acids and dialcohols in virgin olive oil

机译:用于同时测定纯橄榄油中三萜酸和二元醇的基于LC-MS的GC-MS替代方法的开发和验证

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摘要

Pentacyclic triterpenes are minor, but very relevant compounds found in virgin olive oil (VOO). A rapid and reliable LC-MS method for determining the triterpenic acids and dialcohols (after ultrasound assisted extraction) from VOO has been developed, giving an alternative to the widely used GC (FID/MS) methodologies. The analytical parameters of the proposed method were exhaustively checked, establishing limits of detection (from 1 to 95 mu g/l) and quantification, precision (RSD values for inter-day repeatability were found between 4.2 and 7.3% considering area values), trueness (within the range 92.7 and 100.5%) and evaluating possible matrix effect (which was no significant). The method was applied to the analysis of six triterpenic compounds in 11 monovarietal VOOs and the results compared with the quantitative GC-MS data. Moreover, the direct injection (after a simple dilution) of the samples into the LC-MS system was also tested, in an attempt to proffer an even simpler sample treatment. (C) 2017 Elsevier Ltd. All rights reserved.
机译:五环三萜是次要的,但在原始橄榄油(VOO)中发现非常相关的化合物。已经开发了一种快速可靠的LC-MS方法(用于从VOO中测定三萜酸和二元醇(超声辅助萃取后)),为广泛使用的GC(FID / MS)方法提供了一种替代方法。对该方法的分析参数进行了详尽的检查,确定了检测限(从1到95μg/ l)和定量,精度(考虑到面积值,发现日间重复性的RSD值介于4.2和7.3%之间),真实性(在92.7和100.5%的范围内)并评估可能的基质效应(无显着性)。该方法用于分析11种单变量VOO中的6种三萜类化合物,并将结果与​​定量GC-MS数据进行比较。此外,还测试了将样品直接注射(简单稀释后)到LC-MS系统中的方法,以试图提供更简单的样品处理方法。 (C)2017 Elsevier Ltd.保留所有权利。

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