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Extraction of organochlorine pesticides from bee pollen by matrix solid-phase dispersion: Recovery evaluation by GC-MS and method validation

机译:基质固相分散从蜂花粉中提取有机氯农药:GC-MS回收率评估和方法验证

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Recovery studies were done with bee pollen spiked with eight organochlorine pesticides. Matrix solidphase dispersion was used to extract pesticides from bee pollen using octadecyl silica (C18, 0.5 g) as solid support. The co-column material for clean-up (graphitized carbon and primary secondary amine) and the eluting system (acetonitrile or acetonitrile/ethyl acetate) were optimized. Pesticide recoveries were determined by GC-MS-SIM through external calibration curves. The recoveries obtained without co-column and primary secondary amine (PSA) did not differ significantly and were higher than those obtained using graphitized carbon. With PSA used as the co-column, chromatograms with low background, low intensity, and fewer peaks were acquired. Thus, primary secondary amine was used to clean up the pollen extracts. Recoveries were higher than 100 % and precisions were poor for most of the pesticides when acetonitrile/ethyl acetate was used to elute them. Therefore, acetonitrile was selected for the elution of organochlorine pesticides. The final extraction conditions were: C18 (adsorbent), primary secondary amine (co-column), and ACN (eluting solvent). Recoveries obtained ranged from 41 to 101 %.
机译:用掺有八种有机氯农药的蜂花粉进行恢复研究。使用十八烷基二氧化硅(C18,0.5 g)作为固体载体,使用基质固相分散体从蜂花粉中提取农药。优化了用于纯化的共柱材料(石墨化碳和伯仲胺)和洗脱系统(乙腈或乙腈/乙酸乙酯)。通过GC-MS-SIM通过外部校准曲线确定农药的回收率。不使用共柱和伯仲胺(PSA)获得的回收率没有显着差异,并且高于使用石墨化碳获得的回收率。使用PSA作为共柱,可得到背景低,强度低和峰少的色谱图。因此,伯仲胺用于清除花粉提取物。当使用乙腈/乙酸乙酯洗脱大多数农药时,其回收率高于100%,并且精密度很差。因此,选择乙腈洗脱有机氯农药。最终萃取条件为:C18(吸附剂),伯仲胺(共柱)和ACN(洗脱溶剂)。回收率在41%到101%之间。

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