Carrasco-Pancorbo Alegría, Arráez-Román David, Segura-Carretero Antonio, Fernández-Gutiérrez Alberto
Department of Analytical Chemistry, Faculty of Sciences, University of Granada, Spain.
Electrophoresis. 2006 Jun;27(11):2182-96. doi: 10.1002/elps.200500650.
We describe the first analytical method involving SPE and CZE coupled to ESI-IT MS (CZE-ESI-MS) used to identify and characterize phenolic compounds in olive oil samples. The SPE, CZE and ESI-MS parameters were optimized in order to maximize the number of phenolic compounds detected and the sensitivity of their determination. To this end we have devised a detailed method to find the best conditions for CE separation and the detection by MS of the phenolic compounds present in olive oil using a methanol-water extract of Picual extra-virgin olive oil (VOO). Electrophoretic separation was carried out using an aqueous CE buffer system consisting of 60 mM NH(4)OAc at pH 9.5 with 5% of 2-propanol, a sheath liquid containing 2-propanol/water 60:40 v/v and 0.1% v/v triethylamine. This method offers to the analyst the chance to study important phenolic compounds such as phenolic alcohols (tyrosol (TY), hydroxytyrosol (HYTY) and 2-(4-hydroxyphenyl)ethyl acetate), lignans ((+)-pinoresinol and (+)-1-acetoxypinoresinol), complex phenols (ligstroside aglycon (Lig Agl), oleuropein aglycon, their respective decarboxylated derivatives and several isomeric forms of these (dialdehydic form of oleuropein aglycon, dialdehydic form of ligstroside aglycon, dialdehydic form of decarboxymethyl elenolic acid linked to HYTY, dialdehydic form of decarboxymethyl elenolic acid linked to TY) and 10-hydroxy-oleuropein aglycon) and one other phenolic compound (elenolic acid) in extra-VOO by using a simple SPE before CE-ESI-MS analysis.
我们描述了第一种涉及固相萃取（SPE）和毛细管区带电泳（CZE）与电喷雾离子阱质谱联用（CZE-ESI-MS）的分析方法，用于鉴定和表征橄榄油样品中的酚类化合物。对SPE、CZE和ESI-MS参数进行了优化，以最大限度地检测出酚类化合物的数量及其测定的灵敏度。为此，我们设计了一种详细的方法，以找到使用皮夸尔特级初榨橄榄油（VOO）的甲醇-水提取物进行CE分离和通过MS检测橄榄油中存在的酚类化合物的最佳条件。使用由pH 9.5的60 mM醋酸铵和5%的2-丙醇组成的水性CE缓冲系统、含有2-丙醇/水60:40 v/v和0.1% v/v三乙胺的鞘液进行电泳分离。该方法为分析人员提供了一个机会，通过在CE-ESI-MS分析之前使用简单的SPE来研究特级初榨橄榄油中的重要酚类化合物，如酚醇（酪醇（TY）、羟基酪醇（HYTY）和2-(4-羟基苯基)乙酸乙酯）、木脂素（(+)-松脂醇和(+)-1-乙酰氧基松脂醇）、复合酚（橄榄苦苷配基（Lig Agl）、橄榄苦苷配基、它们各自的脱羧衍生物以及这些化合物的几种异构体形式（橄榄苦苷配基的二醛形式、橄榄苦苷配基的二醛形式、与HYTY连接的脱羧甲基橄榄酸的二醛形式、与TY连接的脱羧甲基橄榄酸的二醛形式）和10-羟基橄榄苦苷配基）以及另一种酚类化合物（橄榄酸）。
