qNMRに基づく有機リン系農薬イソキサチオンオキソンの品質管理

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On the quantitative analysis of pesticide residues by LC/MS or GC/MS, the standard samples of pesticides are essential. But most of their purities are not traceable to the International System of Units (SI) and it results in degrading the reliability of analysis data. Therefore, the SI-traceable quality control of pesticide standard samples will be most important. We are developing quantitative nuclear magnetic resonance (qNMR) as one of simple quality control methods that is able to determine the purities or contents with SI traceability. We demonstrated that qNMR was used for the purity determination of two standard samples of isoxathion oxon (IXO), an organophosphorus pesticide. The purities of the two samples were certificated by the manufacture as 96.9% and 98.9% which were calculated from the peak area percentages using GC/FID. On the qNMR spectrum, IXO showed the proton signals in the range of δ 1.0-8.0ppm, and the quantitation was performed by calculating the relative peak area ratios of selected proton signals of the target compound to the known purity and amount of the internal standard, hexadimethylsilane which was calibrated with SI-traceable diethyl phthalate. For this method no reference compound of IXO is needed. The purities of two IXO samples showed 75.4% and 98.5% by qNMR. The relative ratio of the two purities was equivalent to the ratio of IXO peak areas in the two samples observed by GC/MS. This result shows that qNMR does not only lead to SI-traceable purity, but it also will be a rapid and simple SI-traceable quality control method of any pesticides with overall analysis time of only 20min.
2009-04-28

qNMRに基づく有機リン系農薬イソキサチオンオキソンの品質管理

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