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首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >Application of dispersive liquid-liquid microextraction for the determination of aflatoxins B_1, B_2, G_1 and G_2 in cereal products
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Application of dispersive liquid-liquid microextraction for the determination of aflatoxins B_1, B_2, G_1 and G_2 in cereal products

机译:分散液-液微萃取在谷物产品中黄曲霉毒素B_1,B_2,G_1和G_2测定中的应用

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摘要

The application of dispersive liquid-liquid microextraction (DLLME) technique for the rapid analysis of aflatoxins B_1, B_2, G_1 and G_2 in maize, rice and wheat products has been evaluated. After extraction of aflatoxins from cereal matrices with a mixture of methanol/water 8:2 (v/v), the analytes were rapidly transferred from the extract to another small volume of organic solvent, chloroform, by DLLME. Aflatoxins were determined using high performance liquid chromatography with florescence detection and photochemical post-column derivatization. Parameters affecting both extraction and DLLME procedures, such as extraction solvent, type and volume of DLLME extractant, volume of water and salt effect, were systematically investigated and optimized to achieve the best extraction efficiency. Under the optimal experimental conditions, the whole analytical method provides enrichment factors around 2.5 times and detection limits (0.01-0.17μgkg~(-1)) below the maximum levels imposed by current regulation for aflatoxins in cereals and cereal products intended for direct human consumption. Recoveries (67-92%) and repeatability (RSD<10, n=3), tested in three different cereal matrices, meet the performance criteria required by EC Regulation No. 401/2006 for the determination of the levels of mycotoxins in foodstuffs. The proposed method was successfully applied to the analysis of retail cereal products with quantitative results comparable to the immunoaffinity chromatography (IAC). The main advantages of developed method are the simplicity of operation, the rapidity to achieve a very high sample throughput and low cost.
机译:评价了分散液-液微萃取(DLLME)技术在玉米,大米和小麦产品中黄曲霉毒素B_1,B_2,G_1和G_2的快速分析中的应用。用甲醇/水8:2(v / v)的混合物从谷物基质中提取黄曲霉毒素后,通过DLLME将分析物从提取物中快速转移到另一小体积的有机溶剂氯仿中。使用具有荧光检测和光化学柱后衍生作用的高效液相色谱法测定黄曲霉毒素。系统地研究和优化了影响萃取和DLLME程序的参数,例如萃取溶剂,DLLME萃取剂的类型和体积,水量和盐分效应,以实现最佳萃取效率。在最佳实验条件下,整个分析方法可提供约2.5倍的富集因子,且检测限(0.01-0.17μgkg〜(-1))低于现行法规对谷物和拟供人类直接食用的谷物产品中黄曲霉毒素的最大限量。在三种不同的谷物基质中测试的回收率(67-92%)和重复性(RSD <10,n = 3)符合EC法规401/2006所要求的确定食品中真菌毒素水平的性能标准。所提出的方法已成功地应用于零售谷物产品的分析,其定量结果可与免疫亲和色谱法(IAC)媲美。所开发方法的主要优点是操作简单,快速实现非常高的样品通量和低成本。

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