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A Simplified HPLC Procedure for the Determination of Glyphosate in Soybeans Employing Postcolumn Fluorescence Labeling

机译:柱后荧光标记法测定大豆中草甘膦的简化HPLC程序

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摘要

An analytical procedure for residues of the herbicide glyphosate [N-phosphonomethylglycine] in soybeans is described. Extraction of soybeans is performed with 20 mmol/L borate buffer solution. Cleanup is achieved by an ortho-phthalaldehyde-mercaptoethanol (OPA-MERC) reaction followed by application to a dual mini-cartridge column (graphite and octadecyl-bonded silica gel) system, and determination is performed by ion-pair mode high-performance liquid chromatogra- phy employing postcolumn fluorescence labeling of the appropriate primary amine with OPA- MERC. Conversion of glyphosate to a primary amine (presumably ammonia and/or glycine) is achieved postcolumn by oxidation with sodium hypochlorite. Residues can easily be measured at the 0.05 ppm level with recoveries greater than 74/100. The efficiency of the purification and the simplicity of the procedure allow for high sample throughput compared to existing procedures.
机译:描述了大豆中除草剂草甘膦[N-膦酰基甲基甘氨酸]残留的分析程序。大豆的提取是用20 mmol / L硼酸盐缓冲溶液进行的。通过邻苯二甲醛-巯基乙醇(OPA-MERC)反应,然后应用于双微型柱(石墨和十八烷基键合的硅胶)系统进行纯化,并通过离子对模式高性能液体进行测定色谱后,采用OPA-MERC对相应的伯胺进行柱后荧光标记。草甘膦向次要胺(大概是氨和/或甘氨酸)的转化是在柱后通过用次氯酸钠氧化实现的。残留物可以很容易地在0.05 ppm的水平上测定,回收率大于74/100。与现有程序相比,纯化的效率和程序的简单性可实现较高的样品通量。

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