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目前测定大米中杀虫环的农药残留多采用气相色谱方法,样品前处理时试剂需要提纯,既危险又繁琐,目标峰还存在干扰,影响定性;采用液相色谱和液质联用的方法处理样品需使用固相萃取柱,增加了检测成本,也比较费时间,液质联用方法虽然定性比较准确,但其检出限比较高。本文采用溶剂萃取方法处理样品,气质质联用仪测定,样品处理简单,耗材成本低。本方法对仪器条件进行了优化,具有较好的重复性和较低的检出限。测定重复性的标准偏差(RSD)达到4.1%,检出限达到0.8μg/kg,由于本方法较低的检出限,对研究大米中农残杀虫环的降解过程将提供有力的检测手段。
At present, the pesticide residues in rice are mainly determined by gas chromatography. When the sample is pretreated, the reagents need to be purified, which is both dangerous and cumbersome. The target peak still interferes with the quality of the pesticide residues and affects the qualitative determination. Liquid chromatography and liquid chromatography-mass spectrometry Samples need to use solid-phase extraction column, an increase of detection costs, but also more time-consuming, although qualitative and quantitative LC / MS method more accurate, but its detection limit is relatively high. In this paper, solvent extraction method for processing samples, gas quality analyzer, sample processing simple, consumables low cost. The method has been optimized for instrument conditions, has good repeatability and lower detection limit. The standard deviation (RSD) of repeatability was 4.1% and the detection limit was 0.8μg / kg. The low detection limit of this method will provide a powerful means of detecting the degradation process of pesticide ring in rice.