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Rapid Method for Determination of Phosphine Residues in Wheat

机译:小麦中膦残留量的快速测定方法

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摘要

A rapid method for spectrophotometric determination of phosphine residues in wheat has been developed. Phosphine-fumigated wheat kernels were added with 10% sulfuric acid in a gas-tight flask, and phosphine was released into the headspace by microwave irradiation. Phosphine was spectrophotometrically determined after reaction with silver nitrate. A good linearity of the calibration curve was obtained with wheat spiked at levels ranging from 0.035 to 0.230 μg/g with correlation coefficient (r) of 0.9965 and a detection limit of 0.026 μg/g. The total time of analysis was 10 min. Headspace analysis was also performed by micro-gas chromatography (GC) with a thermal conductivity detector (micro-GC-TCD). Results obtained with the spectrophotometric and micro-GC-TCD methods showed good correlations with those obtained with the most widely used GC with nitrogen–phosphorus detector with r values of 0.9940 and 0.9946, respectively.
机译:已经开发了一种快速光度法测定小麦中膦残留量的方法。将磷化氢熏蒸的小麦籽粒在不透气的烧瓶中添加10%的硫酸,然后通过微波辐射将磷化氢释放到顶部空间。与硝酸银反应后,用分光光度法测定了膦。小麦加标浓度范围为0.035至0.230μg/ g,相关系数(r)为0.9965,检出限为0.026μg/ g时,校准曲线具有良好的线性。分析的总时间为10分钟。顶空分析还通过带有热导检测器(micro-GC-TCD)的微型气相色谱(GC)进行。用分光光度法和微型GC-TCD方法获得的结果与使用最广泛的带有氮磷检测器的GC的结果具有良好的相关性,r值分别为0.9940和0.9946。

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