Determination of Squalene in Organic Extra Virgin Olive Oils (EVOOs) by UPLC/PDA Using a Single-Step SPE Sample Preparation
Determination of Squalene in Organic Extra Virgin Olive Oils (EVOOs) by UPLC/PDA Using a Single-Step SPE Sample Preparation
复制标题
使用单步 SPE 样品制备，通过 UPLC/PDA 测定有机特级初榨橄榄油 (EVOO) 中的角鲨烯
作者：
A. Salvo;G. L. La Torre;A. Rotondo;Valentina Mangano;Katia Erminia Casale;Vito Pellizzeri;M. L. Clodoveo;F. Corbo;N. Cicero;G. Dugo
本文采用一种简单、快速的检测方法测定特级初榨橄榄油中的角鲨烯（SQ）。采用高效的单步固相萃取法（SPE）从EVOOs中纯化SQ，并用UPLC-PDA仪器测定其含量。对所采用的技术进行了准确性、线性度、灵敏度和重复性评价。在25 mg L−1和50 mg L−1添加水平下，固相萃取精密度高，平均回收率分别为91.9±0.4和96.3±0.3%。所选色谱条件允许快速SQ测定；事实上，它在0.54 min内分离得很好，分辨率也很好。该方法在50 ~ 500 mg L−1范围内线性良好（R2 = 0.9998）。以0.3 mg L−1的检出限（LOD）评价方法的灵敏度。采用该方法对来自土耳其、突尼斯、西班牙、葡萄牙、希腊、美国、斯洛文尼亚、阿尔巴尼亚、以色列、意大利等33个国家的有机EVOO样品进行SQ测定，并对所得数据进行统计学评价。
In this paper, a simple extraction and fast detection procedure was used to determine squalene (SQ) in extra virgin olive oils (EVOOs). SQ was purified from EVOOs by an efficient single-step solid phase extraction (SPE), and its content was determined using an UPLC-PDA instrument. The adopted technique was evaluated for accuracy, linearity, sensitivity, and repeatability. The precision of the SPE extraction was satisfactory and the mean recoveries were 91.9 ± 0.4 and 96.3 ± 0.3 % for 25 and 50 mg L−1 level of addition, respectively. The selected chromatographic conditions allowed a very fast SQ determination; in fact, it was well separated in ∼0.54 min with good resolution. The UPLC method showed a good linearity in the range 50–500 mg L−1 (R2 = 0.9998). Method sensitivity was evaluated by measuring the limits of detection (LOD) that was 0.3 mg L−1. The method was utilized for SQ determination in 33 different organic EVOO samples, coming from different countries (Turkey, Tunisia, Spain, Portugal, Greece, USA, Slovenia, Albania, Israel, Italy) and the data were statistically evaluated.