Department of Chemistry, Building of Pharmaceutical Sciences, University of Florence , Via Ugo Schiff 6, 50019 Sesto Fiorentino (FI), Firenze, Italy.
J Agric Food Chem. 2014 Dec 31;62(52):12529-35. doi: 10.1021/jf503769s. Epub 2014 Dec 19.
In the present study an HPLC-DAD method was developed for the determination of the main carotenoid, zeaxanthin dipalmitate, in the fruits of Lycium barbarum. The aim was to develop and optimize an extraction protocol to allow fast, exhaustive, and repeatable extraction, suitable for labile carotenoid content. Use of liquid N2 allowed the grinding of the fruit. A step of ultrasonication with water removed efficiently the polysaccharides and enabled the exhaustive extraction of carotenoids by hexane/acetone 50:50. The assay was fast and simple and permitted the quality control of a large number of commercial samples including fruits, juices, and a jam. The HPLC method was validated according to ICH guidelines and satisfied the requirements. Finally, the overall method was validated for precision (% RSD ranging between 3.81 and 4.13) and accuracy at three concentration levels. The recovery was between 94 and 107% with RSD values <2%, within the acceptable limits, especially if the difficulty of the matrix is taken into consideration.
本研究建立了高效液相色谱-二极管阵列检测法（HPLC-DAD），用于测定枸杞果实中的主要类胡萝卜素二棕榈酸酯叶黄素。目的是开发并优化一种提取方案，以实现快速、彻底和可重复的提取，适用于不稳定类胡萝卜素含量的分析。使用液氮研磨可以粉碎果实。通过水超声处理的步骤可以有效地去除多糖，并通过正己烷/丙酮（50:50）彻底提取类胡萝卜素。该分析方法快速简单，可用于控制大量商业样品（包括水果、果汁和果酱）的质量。HPLC 方法根据 ICH 指南进行了验证，满足要求。最后，在三个浓度水平上对整个方法的精密度（%RSD 范围在 3.81 到 4.13 之间）和准确度进行了验证。回收率在 94%到 107%之间，RSD 值<2%，在可接受的范围内，尤其是考虑到基质的难度。
