该试验自主研发磁性纳米粒子负载十八烷胺功能化介孔碳复合材料,基于QuEChERS技术联合气相色谱-质谱联用仪开发一种绿叶菜有机磷农药残留量快速检测样品前处理方法。该磁性介孔复合材料的表面结构特征通过透射电子显微镜、X-射线衍射、磁强计、氮气吸附-脱附等手段进行了表征。实验结果表明,与传统的净化剂相比,该磁性介孔材料能够很好地消除基质干扰,提高检测效率,操作简单。绿叶菜基质中16种有机磷农药残留量在0.02~0.25 μg/mL具有良好的线性关系,相关系数(R2)在0.994 3~0.999 7,在0.02、0.05、0.10 mg/kg添加水平下,绿叶菜基质中16种有机磷农药平均回收率在81.3%~94.0%,相对标准偏差＜10%,检出限为0.01~0.08 μg/mL。将该方法应用于实际绿叶菜样品的检测,结果显示所有绿叶菜样品均符合有机磷农药最大残留限量标准。该方法具有灵敏度高、通用性强、准确度高、稳定性好、经济环保等优点,适用于其他蔬菜及水果中农药残留量检测样品前处理中。
In this study, magnetic nanoparticles loaded octadecylamine functionalized mesoporous carbon composites were independently developed and a sample pretreatment method for rapid detection of organophosphorus pesticide residues in green leafy vegetables based on QuEChERS technology and gas chromatography-mass spectrometry was developed. The surface structure of the magnetic mesoporous composite was characterized by transmission electron microscopy, X-ray diffraction, magnetometer and nitrogen adsorption-desorption. The experimental results showed that compared with the traditional purification agent, the magnetic mesoporous material could eliminate the matrix interference, improve the detection efficiency. In addition, the operation was simple. The residues of 16 organophosphorus pesticides in green leafy vegetables ranged from 0.02-0.25 μg/mL with the correlation coefficient (R2) of 0.994 3-0.999 7. The average recoveries of 16 organophosphorus pesticides in green leafy vegetables were 81.3%-94.0% at the levels of 0.02, 0.05 and 0.10 mg/kg, and the relative standard deviations were less than 10%. The detection limits were 0.01-0.08 μg/mL. Then, the method was applied to detect green leafy vegetables. The results showed that all green leafy vegetables met the maximum residue limit of organophosphorus pesticides. This method has the advantages of high sensitivity, strong universality, high accuracy, good stability, economic and environmental protection, and is suitable for the pretreatment of pesticide residues in other vegetables and fruits.
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