Determination of nitenpyram and its metabolites in agricultural products by using hydrophilic interaction liquid chromatography-tandem mass spectrometry
Determination of nitenpyram and its metabolites in agricultural products by using hydrophilic interaction liquid chromatography-tandem mass spectrometry
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DOI：
10.1584/jpestics.d12-049
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发表时间：
2013-02
影响因子：
2.4
通讯作者：
Tatsu Yoshida;H. Murakawa;K. Toda
中科院分区：
文献类型：
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作者：
Tatsu Yoshida;H. Murakawa;K. Toda
研究了一种快速、简便测定烟碱类农药烯啶虫胺及其代谢物CPMA和CPMF的方法。通过简单超声提取，然后亲水作用液相色谱-串联质谱法（HILIC-MS/MS）单独和同时测定三种化合物。使用未改性的硅胶柱获得良好的色谱图。各化合物的线性关系良好（R2>0.999），在5g农产品样品中的检出限（S/N=3）为0.24-0.36 μg/kg（烯啶虫胺），0.12-0.19 μg/kg（CPMA），0.13-0.18 μg/kg（CPMF）。甜椒、橘子橙子、洋葱和糙米的回收率在93.0-106.6%之间。对于污染样品，所提出的方法的数据与烯啶虫胺的HPLC-UV数据和总的CPMA和CPMF的衍生化，然后用气相色谱-火焰离子检测器。
A simple and rapid method for the measurement of a neonicotinoid pesticide, nitenpyram, and its metabolites, CPMA and CPMF, was investigated. The three compounds were determined individually and simultaneously by simple ultrasonic extraction followed by hydrophilic interaction liquid chromatography-tandem mass spectrometry (HILIC-MS/MS). Good chromatograms were obtained using a non-modified silica gel column. The calibration curves were straight (R2>0.999) for each compound; they were 0.002–2 mg/kg for 5 g of agricultural product sample with limits of detection (S/N=3) of 0.24–0.36 μg/kg (nitenpyram), 0.12–0.19 μg/kg (CPMA), and 0.13–0.18 μg/kg (CPMF). Good recoveries were obtained for sweet pepper, mandarin orange, onion, and brown rice (93.0–106.6% in recovery). For contaminated samples, data by the presented method agreed well with nitenpyram data by HPLC-UV and the total of CPMA and CPMF by derivatization followed by gas chromatography-flame thermionic detection.