Department of Analytical Chemistry, Faculty of Sciences, University of Granada, Avenida Fuentenueva s/n, 18071 Granada, Spain; Research and Development Functional Food Centre (CIDAF), Bioregión Building, Health Science Technological Park, Avda. Del Conocimiento s/n, 18016 Granada, Spain.
Department of Analytical Chemistry, Faculty of Sciences, University of Granada, Avenida Fuentenueva s/n, 18071 Granada, Spain; Research and Development Functional Food Centre (CIDAF), Bioregión Building, Health Science Technological Park, Avda. Del Conocimiento s/n, 18016 Granada, Spain.
Talanta. 2015 Jan;132:929-38. doi: 10.1016/j.talanta.2014.10.049. Epub 2014 Oct 31.
A new method based on nano-liquid chromatography coupled to time-of-flight mass spectrometry (nano-LC-TOF-MS) using lock-mass calibration was developed to facilitate the accurate and routine characterization and quantification of phenolic compounds. Thus, it was applied to study cranberry syrups, in which, using negative ionization mode, a total of nine phenolic compounds were unequivocally identified using standards and 38 tentatively taking into account their retention time, accurate mass (errors<5 ppm) data and isotope pattern, as well as literature. Among them, 13 compounds, belonging to flavonols and iridoids conjugated with phenolic acids, were reported for first time in cranberry or cranberry based-products. The analytical method was also validated using chlorogenic acid, p-coumaric acid, (+)-catechin, (-)-epicatechin, procyanidin A2, quercetin 3-O-glucoside, quercetin 3-O-rhamnoside, quercetin, and myricetin standards. In this way, the analytical method showed adequate linearity, with R(2) above 0.99, and acceptable values of intra- and inter-day repeatability of the retention time and peak area. The detection limits and quantification were between 1.0-15.6 ng mL(-1) and 2.0-62.5 ng mL(-1), respectively. The method can be extended to characterize phenolic compounds in other food and plant matrices, and as well biological samples.
基于纳米液相色谱-飞行时间质谱联用（nano-LC-TOF-MS），采用内标法定量，建立了一种新方法，用于准确、常规地对酚类化合物进行鉴定和定量分析。本方法应用于蔓越莓糖浆的分析，在负离子模式下，共鉴定出 9 种酚类化合物，其中 13 种化合物为首次在蔓越莓或蔓越莓制品中发现，通过标准品和保留时间、精确质量（误差<5 ppm）数据和同位素模式，以及文献检索，对这些化合物进行了定性分析。其中，13 种化合物属于黄酮醇和与酚酸共轭的环烯醚萜，同时对绿原酸、对香豆酸、（+）-儿茶素、（-）-表儿茶素、原花青素 A2、槲皮苷 3-O-葡萄糖苷、槲皮苷 3-O-鼠李糖苷、槲皮素和杨梅素标准品进行了定量分析。结果表明，该方法具有良好的线性关系（R2>0.99），日内和日间精密度良好，保留时间和峰面积的相对标准偏差均小于 10%。该方法的检测限和定量限分别为 1.0-15.6 ng·mL-1 和 2.0-62.5 ng·mL-1。该方法可扩展用于其他食品和植物基质以及生物样品中酚类化合物的分析。
