Karami-Osboo Rouhollah, Miri Ramin, Javidnia Katayoun, Kobarfard Farzad, AliAbadi Mohammad Hossein Shojaee, Maham Mehdi
Medicinal and Natural Products Chemistry Research Centre, Shiraz University of Medical Sciences, Shiraz, Iran.
Department of Medicinal Chemistry, School of Pharmacy, Shaheed Beheshti Medical University, P.O. Box 14155-6153, Tehran, Iran.
J Food Sci Technol. 2015 Apr;52(4):2440-5. doi: 10.1007/s13197-013-1215-4. Epub 2013 Dec 12.
A method based on dispersive liquid-liquid microextraction (DLLME) was developed for the quantitative extraction of Ochratoxin A (OTA) from raisin samples. The influence of various parameters on the recovery of OTA such as type and volume of DLLME extractant, centrifuging and sonication time, also volume of deionized water was investigated. Recovery values under the optimum conditions were between 68.6 and 85.2 %, the inner and intra-day precision expressed as relative standard deviation (RSD%, n = 3), were less than 15 % at spiking levels of 2.5-30 μg kg(-1). Linearity was studied from 0.5 to 30 μg L(-1), and the limits of detection (LOD) and quantification (LOQ) were 0.7 and 2.0 μg kg(-1), respectively. Real samples were analyzed by DLLME method and compared with confirmative immunoaffinity Column Chromatography (IAC) clean-up. Low cost, simplicity of operation, speed and minimum consumption of organic solvent were the main advantages of proposed method. The mean contamination of samples was 0.88 μg kg(-1) that was lower than European Legal Limit.
建立了一种基于分散液液微萃取（DLLME）的方法，用于从葡萄干样品中定量萃取赭曲霉毒素A（OTA）。研究了各种参数对OTA回收率的影响，如DLLME萃取剂的类型和体积、离心和超声处理时间以及去离子水的体积。在最佳条件下，回收率在68.6%至85.2%之间，在2.5-30μg kg(-1)的加标水平下，日内和日间精密度以相对标准偏差（RSD%，n = 3）表示，均小于15%。线性范围为0.5至30μg L(-1)，检测限（LOD）和定量限（LOQ）分别为0.7和2.0μg kg(-1)。采用DLLME法对实际样品进行分析，并与确证性免疫亲和柱色谱（IAC）净化法进行比较。该方法的主要优点是成本低、操作简单、速度快且有机溶剂消耗最少。样品的平均污染量为0.88μg kg(-1)，低于欧洲法定限量。
