Department of Analytical Chemistry, Faculty of Sciences, University of Granada, c/ Fuentenueva s/n, E-18071 Granada, Spain.
J Chromatogr A. 2011 Feb 18;1218(7):959-71. doi: 10.1016/j.chroma.2010.12.014. Epub 2010 Dec 13.
A new analytical approach based on gas chromatography coupled to atmospheric pressure chemical ionization-time of flight mass spectrometry was evaluated for its applicability for the analysis of phenolic compounds from extra-virgin olive oil. Both chromatographic and MS parameters were optimized in order to improve the sensitivity and to maximize the number of phenolic compounds detected. We performed a complete analytical validation of the method with respect to its linearity, sensitivity, precision, accuracy and possible matrix effects. The LODs ranged from 0.13 to 1.05ppm for the different tested compounds depending on their properties. The RSDs for repeatability test did not exceed 6.07% and the accuracy ranged from 95.4% to 101.5%. To demonstrate the feasibility of our method for analysis of real samples, we analyzed the extracts of three different commercial extra-virgin olive oils. We have identified unequivocally a number of phenolic compounds and obtained quantitative information for 21 of them. In general, our results show that GC-APCI-TOF MS is a flexible platform which can be considered as an interesting tool for screening, structural assignment and quantitative determination of phenolic compounds from virgin olive oil.
一种基于气相色谱-大气压化学电离-飞行时间质谱联用的新分析方法，用于分析特级初榨橄榄油中的酚类化合物。为了提高灵敏度和最大限度地增加检测到的酚类化合物数量，对色谱和 MS 参数进行了优化。对该方法的线性、灵敏度、精密度、准确度和可能的基质效应进行了全面的分析验证。不同测试化合物的 LOD 值范围为 0.13 至 1.05ppm，具体取决于其性质。重复性测试的 RSD 不超过 6.07%，准确度范围为 95.4%至 101.5%。为了证明我们的方法用于分析实际样品的可行性，我们分析了三种不同商业特级初榨橄榄油的提取物。我们已经明确鉴定了一些酚类化合物，并获得了其中 21 种的定量信息。总的来说，我们的结果表明，GC-APCI-TOF MS 是一种灵活的平台，可以被认为是筛选、结构鉴定和定量测定橄榄油中酚类化合物的一种有趣工具。
