Fan Chen, Cao Xueli, Liu Man, Wang Wei
Beijing Technology and Business University, Beijing Key Lab of Food Quality and Safety, Beijing 100048, China; Beijing Centre for Physical and Chemical Analysis, Beijing 100089, China.
Beijing Technology and Business University, Beijing Key Lab of Food Quality and Safety, Beijing 100048, China.
J Chromatogr A. 2016 Mar 4;1436:133-40. doi: 10.1016/j.chroma.2016.01.069. Epub 2016 Jan 29.
Alternariol (AOH), alternariol monomethyl ether (AME), and tenuazonic acid (TeA) are some of the main Alternaria mycotoxins that can be found as contaminants in food materials. The objective of this study was to develop a pretreatment method with countercurrent chromatography (CCC) for enrichment and cleanup of trace Alternaria mycotoxins in food samples prior to high-performance liquid chromatography (HPLC) analysis. An Analytical CCC instrument with a column volume 22.5mL was used, and a two-phase solvent system composed of ethyl acetate and water modified with 6% [HOOMIM][Cl] in mass to volume ratio was selected. Under the optimized CCC operation conditions, trace amounts of AOH, AME, and TeA in large volume of liquid sample were efficiently extracted and enriched in the stationary phase, and then eluted out just by reversing the stationary phase as mobile phase in the opposite flowing direction tail-to-head. The enrichment and elution strategies are unique and can be fulfilled online with high enrichment factors (87-114) and high recoveries (81.14-110.94%). The method has been successively applied to the determination of Alternaria mycotoxins in real apple juice and wine samples with the limits of detection (LOD) in the range of 0.03-0.14μgL(-1). Totally 12 wine samples and 15 apple juice samples from the local market were analyzed. The detection rate of AOH and AME in both kinds of the samples were more than 50%, while TeA was found in relatively high level of 1.75-49.61μgL(-1) in some of the apple juice samples. The proposed method is simple, rapid, and sensitive and could also be used for the analysis and monitoring of Alternaria mycotoxin in other food samples.
交链孢酚(AOH)、交链孢酚单甲醚(AME)和细交链孢菌酮酸(TeA)是一些主要的链格孢属霉菌毒素,可在食品原料中作为污染物被发现。本研究的目的是开发一种采用逆流色谱(CCC)的预处理方法,用于在高效液相色谱(HPLC)分析之前对食品样品中的痕量链格孢属霉菌毒素进行富集和净化。使用了一台柱体积为22.5mL的分析型CCC仪器,并选择了由乙酸乙酯和用质量体积比为6%的[HOOMIM][Cl]改性的水组成的两相溶剂系统。在优化的CCC操作条件下,大量液体样品中的痕量AOH、AME和TeA在固定相中被高效萃取和富集,然后通过将固定相反转为流动相并以相反的头尾流动方向洗脱出来。富集和洗脱策略独特,可以在线完成,具有高富集因子(87 - 114)和高回收率(81.14 - 110.94%)。该方法已成功应用于实际苹果汁和葡萄酒样品中链格孢属霉菌毒素的测定,检测限(LOD)在0.03 - 0.14μg L⁻¹范围内。共分析了来自当地市场的12个葡萄酒样品和15个苹果汁样品。两种样品中AOH和AME的检出率均超过50%,而在一些苹果汁样品中TeA的含量相对较高,为1.75 - 49.61μg L⁻¹。所提出的方法简单、快速且灵敏,也可用于其他食品样品中链格孢属霉菌毒素的分析和监测。