Mencin Marjeta, Mikulic-Petkovsek Maja, Veberič Robert, Terpinc Petra
Department of Food Science and Technology, Biotechnical Faculty, University of Ljubljana, Jamnikarjeva 101, SI-1111 Ljubljana, Slovenia.
Department of Agronomy, Biotechnical Faculty, University of Ljubljana, Jamnikarjeva 101, SI-1111 Ljubljana, Slovenia.
Antioxidants (Basel). 2021 Jul 5;10(7):1085. doi: 10.3390/antiox10071085.
A solid-phase extraction (SPE) technique was developed and optimised for isolation and concentration of extractable and bound phenolic acids from germinated spelt seeds, for analysis by liquid chromatography-mass spectrometry. Samples initially underwent solvent extraction under different conditions to maximise the yield of phenolic antioxidants. Optimal extraction conditions for extractable phenolics were absolute methanol as solvent, sample-to-methanol ratio 1:9, and reconstitution in non-acidified water. The bound phenolics were extracted from sample pellets using hydrolysis with 2 M NaOH, acidification of the hydrolysate with formic acid, and simultaneous isolation and purification using Strata X polymeric RP tubes. Compared to liquid-liquid extraction, this direct SPE protocol has significant advantages in terms of higher extraction efficiencies of total and individual phenolics and their antioxidant activities. These data suggest that direct SPE represents a rapid and reliable method for quantitative analysis of both the extractable and the commonly overlooked bound phenolics in seeds.
开发并优化了一种固相萃取(SPE)技术,用于从发芽的斯佩尔特种子中分离和浓缩可提取和结合的酚酸,以便通过液相色谱 - 质谱法进行分析。样品首先在不同条件下进行溶剂萃取,以最大化酚类抗氧化剂的产量。可提取酚类的最佳萃取条件为:以无水甲醇为溶剂,样品与甲醇比例为1:9,并在非酸化水中复溶。使用2 M NaOH水解从样品颗粒中提取结合酚类,用甲酸酸化水解产物,并使用Strata X聚合物反相管同时进行分离和纯化。与液 - 液萃取相比,这种直接SPE方案在总酚和单个酚类及其抗氧化活性的更高萃取效率方面具有显著优势。这些数据表明,直接SPE是一种快速可靠的方法,可用于定量分析种子中可提取的以及通常被忽视的结合酚类。