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Rapid method based on immunoassay for determination of paraquat residues in wheat, barley and potato

机译:基于免疫分析的快速方法测定小麦,大麦和马铃薯中的百草枯残留量

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The detection of bipyridine herbicides residues in food samples is hampered due to their particular physico-chemical features, which requires the application of specific extraction and analytical procedures, which disqualifies them from being incorporated into the multi-residue methods (MRMs). There is a need for alternative robust and efficient analytical screening methods, and in this respect, we present here a fast and reliable immunochemical analytical procedure for the detection of paraquat (PQ)residues in food samples, particularly potato, barley and wheat. The procedure involves the extraction with 1 N HCI:MeOH at 80 C, followed by centrifugation and filtration, and the extracts can be directly measured by a microplate-based ELISA without any other sample treatment or clean-up, except from buffering the solution and adjusting the pH. Selective polyclonal antibodies, were raised against N-(4-carboxypent-l-yl)-N'-methyl bipyridilium acid (hapten PQ1), and used to establish a high sensitive immunochemical analytical assay, able to measure simultaneously many samples. Under these conditions the accuracy is very good, with almost quantitative recoveries. The non-specific interferences caused by the matrix are negligible for the case of potato and wheat, while for barley it is necessary to further dilute the extract or using a negative certified extract to build the standard calibration curve. The method of extraction consisted in acidic extraction and after a dilution is able to be measured. The analysis method results simply, achieving good detectabilities. The limits of detection (LODs) achieved were between 0.037 ± 0.01 mug kg~(-1) in wheat, 0.71 ± 0.3 ug kg~(-1) in barley and 0.56 ± 0.10 mug kg~(-1) in potatoes, values that are far below the Maximum Residue Level (20 mug kg~(-1)) established by the EU policies for paraquat residues in these foodstuff products. The results demonstrate the high potential of these methods as screening tools for food safety and inspection controls.
机译:食品样品中联吡啶除草剂残留物的检测由于其特殊的理化特性而受阻,这需要应用特定的提取和分析程序,这使它们无法纳入多残留方法(MRM)。需要替代的鲁棒且有效的分析筛选方法,在这方面,我们在此提出一种快速可靠的免疫化学分析程序,用于检测食品样品(尤其是马铃薯,大麦和小麦)中的百草枯(PQ)残留。该程序涉及在80°C下用1 N HCl:MeOH萃取,然后进行离心和过滤,并且可以通过基于微孔板的ELISA直接测量萃取物,而无需进行任何其他样品处理或纯化,除了可以缓冲溶液和调节pH值。产生了针对N-(4-羧基戊-1-基)-N'-甲基联吡啶酸(半抗原PQ1)的选择性多克隆抗体,并用于建立高灵敏的免疫化学分析试剂盒,能够同时测量许多样品。在这些条件下,精度非常好,几乎可以定量回收。对于马铃薯和小麦,由基质引起的非特异性干扰可以忽略不计,而对于大麦,则有必要进一步稀释提取物或使用阴性认证提取物来建立标准校正曲线。提取方法包括酸性提取,稀释后即可测定。分析方法结果简单,可实现良好的可检测性。达到的检出限(LOD)在小麦中为0.037±0.01杯kg〜(-1),在大麦中为0.71±0.3 ug kg〜(-1),在土豆中为0.56±0.10杯kg〜(-1)远低于欧盟针对这些食品中百草枯残留量政策制定的最大残留量水平(20马克杯〜(-1))。结果证明了这些方法作为食品安全和检验控制筛选工具的巨大潜力。

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