Impellizzeri John, Lin Jianming
Firmenich Inc., P.O. Box 5880, Princeton, New Jersey 08543, USA.
J Agric Food Chem. 2006 May 3;54(9):3204-8. doi: 10.1021/jf052870b.
A high-performance liquid chromatography (HPLC) method was developed to quantitatively analyze oleocanthal in extra virgin olive oils. Oleocanthal, a deacetoxy ligstroside aglycone, is known to be responsible for the back of the throat irritation of olive oils and to have probated antiinflamatory activity. Oleocanthal was isolated from small amounts of olive oil sample (1 g) by liquid-liquid extraction. Hexane-acetonitrile was found to be the best solvent system to extract oleocanthal from the oil matrix. The solvent extract was analyzed by reversed-phase HPLC with UV detection at 278 nm. Chromatogaphic separation of oleocanthal from other extracted compounds and of the two geometric isomers of oleocanthal was achieved by an elution gradient with acetonitrile and water. Both the external standard calibration curve and the internal standard calibration curve were established, and quantitation using both calibration curves gave essentially the same result. The reproducibility (RSD = 4.7%), recovery (> 95%), and limit of quantitation (< 1 microg/g) were also determined. Concentrations of oleacanthal in 10 selected throat-burning extra virgin olive oils were determined using the method (ranged from 22 to 190 microg/g) with external standard calibration.
建立了一种高效液相色谱（HPLC）方法，用于定量分析特级初榨橄榄油中的油橄榄苦素。油橄榄苦素是一种脱乙酰氧基橄榄苦苷苷元，已知它会导致橄榄油对喉咙后部产生刺激，并且具有已证实的抗炎活性。通过液 - 液萃取从少量橄榄油样品（1 g）中分离出油橄榄苦素。发现己烷 - 乙腈是从油基质中萃取油橄榄苦素的最佳溶剂体系。溶剂萃取物通过反相HPLC在278 nm处进行紫外检测分析。通过乙腈和水的洗脱梯度实现了油橄榄苦素与其他萃取化合物以及油橄榄苦素的两种几何异构体的色谱分离。建立了外标校准曲线和内标校准曲线，使用这两种校准曲线进行定量得到的结果基本相同。还测定了重现性（RSD = 4.7%）、回收率（> 95%）和定量限（< 1 μg/g）。使用该方法（外标校准）测定了10种选定的有喉咙灼烧感的特级初榨橄榄油中油橄榄苦素的浓度（范围为22至190 μg/g）。
