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Determination of Aflatoxins in Rice Samples by Ultrasound-Assisted Matrix Solid-Phase Dispersion

机译:超声辅助基质固相分散法测定大米中的黄曲霉毒素

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This work describes the application of ultrasound-assisted matrix solid-phase dispersion as an extraction and sample preparation approach for aflatoxins (B-1, B-2, G(1) and G(2)) and subsequent determination of them by high-performance liquid chromatography-fluorescence detection. A Box-Behnken design in combination with response surface methodology was used to determine the affecting parameters on the extraction procedure. The influence of different variables including type of dispersing phase, sample-to-dispersing phase ratio, type and quantity of clean-up phase, ultrasonication time, ultrasonication temperature, nature and volume of the elution solvent was investigated in the optimization study. C18, primary-secondary amine (PSA) and acetonitrile were selected as dispersing phase, clean-up phase and elution solvent, respectively. The obtained optimized values were sample-to-dispersing phase ratio of 1 : 1, 60 mg of PSA, 11 min ultrasonication time, 30 degrees C ultrasonication temperature and 4 mL acetonitrile. Under the optimal conditions, the limits of detection were ranged from 0.09 to 0.14 ng g(-1) and the precisions [relative standard deviation (RSD%)] were <8.6%. The recoveries of the matrix solid-phase dispersion process ranged from 78 to 83% with RSD <10% in all cases. Finally, this method was successfully applied to the extraction of trace amounts of aflatoxins in rice samples.
机译:这项工作描述了超声辅助基质固相分散体作为黄曲霉毒素(B-1,B-2,G(1)和G(2))的提取和样品制备方法的应用,以及随后通过高通量法对其进行测定的方法。高效液相色谱-荧光检测。 Box-Behnken设计与响应面方法相结合,用于确定提取过程中的影响参数。在优化研究中,研究了分散相类型,样品与分散相之比,净化相的类型和数量,超声处理时间,超声处理温度,洗脱溶剂的性质和体积等不同变量的影响。选择C18,伯-仲胺(PSA)和乙腈分别作为分散相,净化相和洗脱溶剂。获得的最佳值是样品与分散相的比例为1:1、60 mg PSA,11分钟超声处理时间,30℃超声处理温度和4 mL乙腈。在最佳条件下,检出限为0.09至0.14 ng g(-1),精度[相对标准偏差(RSD%)] <8.6%。在所有情况下,基体固相分散工艺的回收率在78%至83%之间,RSD <10%。最终,该方法成功应用于大米样品中痕量黄曲霉毒素的提取。

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