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改性磁性纳米粒子用于有机农药萃取和富集的研究

发布时间:2019-05-22 13:24
【摘要】:随着农业化大生产的快速发展,农药的广泛使用不可避免,残留在自然界中的农药对动植物和人类的健康造成了影响,因而受到广泛关注。多数有机农药属于脂溶性,难以降解并且长期残留于环境体系,如水、空气、土壤和食品中。以氨基甲酸酯、拟除虫菊酯类、有机磷类农药和磺酰脲类的残留较为广泛。残留的农药可以通过食物链蓄积放大影响动植物及人类健康,这些特点使其危害作用相当显著。如今,随着人们对高品质生活质量的追求,针对农药残留的萃取和分离已有越来越多的研究出现,因此发展灵敏廉价、高效省时、环境友好和简单易行的分析检测方法将是大势所趋。本文合成了具有表面修饰的磁性纳米粒子,并采用磁性固相萃取的方法将其应用于有机农药样品的前处理过程中。将不同活性材料和磁性纳米粒子相结合,将增强对目标物的萃取和富集效果,使方法更加高效简便、省时节能、环境友好,而合成的材料使用范围广泛,常用于环境样品的前处理领域。1.建立磁性纳米粒子-疏水离子液体磁性固相萃取法,对合成的功能化磁性纳米材料进行了元素分析、傅里叶变换红外光谱等一系列表征,结果证明成功键合。将单因素实验用于优化最佳萃取条件,富集和萃取三种有机磷类农药。线性相关系数R20.999,三种目标物的相对标准偏差(RSD)为3.6-5.8%,三种目标物的定量限(LOQ)和检测限(LOD)分别为1.699-3.144μg mL-1和0.543-0.945μg mL-1。将此方法用于实际环境水样中有机磷类农药的富集和检测,获得了满意的结果。2.建立磁性纳米粒子-聚合离子液体分散固相萃取法,用于土壤中三种磺酰脲类农药的富集和萃取。通过单因素实验,对吸附剂用量、洗脱剂种类和用量、萃取时间等因素进行考察,探索最佳萃取条件。实验于最优条件下进行,线性相关系数R20.999,三种目标物的相对标准偏差(RSD)为3.2-4.5%,三种磺酰脲类农药检测限和定量限分别为1.62-2.94μg L-1和5.4-9.8μg L-1之间。将此方法用于实际土壤中磺酰脲类农药的富集和检测,获得了满意的结果。3.依据共沉淀法和溶剂热法合成不同粒径的磁性纳米粒子,继而将聚吡咯包覆在上述材料表面,结合磁性固相萃取-气相色谱-质谱检测的方法,富集和检测中药样品中四种拟除虫菊酯类农药。将单因素实验用于优化最佳萃取条件。在最优条件下,线性相关系数R20.99,相对标准偏差(RSD)为2.6-3.8%,目标物检测限和定量限分别为0.016-0.064μgL-1和0.053-0.211μgL-1。将此方法用于市售中药样品中拟除虫菊酯类农药的富集和检测,获得了满意的结果。
[Abstract]:With the rapid development of agricultural mass production, the wide use of pesticides is inevitable, the pesticide residues in nature have had an impact on the health of animals and plants and human beings, so it has been widely concerned. Most organic pesticides are fat-soluble, difficult to degrade and remain in environmental systems for a long time, such as water, air, soil and food. Carbamate, pyrethroid, organophosphorus pesticides and sulfonylurea residues are more extensive. The residual pesticides can affect the health of animals and plants and human beings through the accumulation of food chain, and these characteristics make their harmful effects quite significant. Nowadays, with the pursuit of high quality of life, more and more studies have appeared on the extraction and separation of pesticide residues, so the development is sensitive, cheap, efficient and time-saving. Environmentally friendly and simple analytical and testing methods will be the general trend of the times. In this paper, magnetic nanoparticles with surface modification were synthesized and applied to the pretreatment of organic pesticide samples by magnetic solid phase extraction. The combination of different active materials and magnetic nanoparticles will enhance the extraction and enrichment of the target, make the method more efficient and simple, time-saving and energy-saving, environmentally friendly, and the synthesized materials are widely used. It is often used in the field of pretreatment of environmental samples. Magnetic solid phase extraction (SPME) of magnetic nanoparticles and hydrophobic ionic liquids was established. The functional magnetic nanomaterials were characterized by elemental analysis and Fourier transform infrared spectroscopy (FTIR). The results showed that the bonding was successful. The single factor experiment was used to optimize the optimum extraction conditions, enrich and extract three organophosphorus pesticides. The linear correlation coefficient R20.999, the relative standard deviation (RSD) of the three targets is 3.6 鈮,

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