【摘要】：隨著農(nóng)業(yè)化大生產(chǎn)的快速發(fā)展,農(nóng)藥的廣泛使用不可避免,殘留在自然界中的農(nóng)藥對動植物和人類的健康造成了影響,因而受到廣泛關(guān)注。多數(shù)有機(jī)農(nóng)藥屬于脂溶性,難以降解并且長期殘留于環(huán)境體系,如水、空氣、土壤和食品中。以氨基甲酸酯、擬除蟲菊酯類、有機(jī)磷類農(nóng)藥和磺酰脲類的殘留較為廣泛。殘留的農(nóng)藥可以通過食物鏈蓄積放大影響動植物及人類健康,這些特點(diǎn)使其危害作用相當(dāng)顯著。如今,隨著人們對高品質(zhì)生活質(zhì)量的追求,針對農(nóng)藥殘留的萃取和分離已有越來越多的研究出現(xiàn),因此發(fā)展靈敏廉價、高效省時、環(huán)境友好和簡單易行的分析檢測方法將是大勢所趨。本文合成了具有表面修飾的磁性納米粒子,并采用磁性固相萃取的方法將其應(yīng)用于有機(jī)農(nóng)藥樣品的前處理過程中。將不同活性材料和磁性納米粒子相結(jié)合,將增強(qiáng)對目標(biāo)物的萃取和富集效果,使方法更加高效簡便、省時節(jié)能、環(huán)境友好,而合成的材料使用范圍廣泛,常用于環(huán)境樣品的前處理領(lǐng)域。1.建立磁性納米粒子-疏水離子液體磁性固相萃取法,對合成的功能化磁性納米材料進(jìn)行了元素分析、傅里葉變換紅外光譜等一系列表征,結(jié)果證明成功鍵合。將單因素實(shí)驗(yàn)用于優(yōu)化最佳萃取條件,富集和萃取三種有機(jī)磷類農(nóng)藥。線性相關(guān)系數(shù)R20.999,三種目標(biāo)物的相對標(biāo)準(zhǔn)偏差(RSD)為3.6-5.8%,三種目標(biāo)物的定量限(LOQ)和檢測限(LOD)分別為1.699-3.144μg mL-1和0.543-0.945μg mL-1。將此方法用于實(shí)際環(huán)境水樣中有機(jī)磷類農(nóng)藥的富集和檢測,獲得了滿意的結(jié)果。2.建立磁性納米粒子-聚合離子液體分散固相萃取法,用于土壤中三種磺酰脲類農(nóng)藥的富集和萃取。通過單因素實(shí)驗(yàn),對吸附劑用量、洗脫劑種類和用量、萃取時間等因素進(jìn)行考察,探索最佳萃取條件。實(shí)驗(yàn)于最優(yōu)條件下進(jìn)行,線性相關(guān)系數(shù)R20.999,三種目標(biāo)物的相對標(biāo)準(zhǔn)偏差(RSD)為3.2-4.5%,三種磺酰脲類農(nóng)藥檢測限和定量限分別為1.62-2.94μg L-1和5.4-9.8μg L-1之間。將此方法用于實(shí)際土壤中磺酰脲類農(nóng)藥的富集和檢測,獲得了滿意的結(jié)果。3.依據(jù)共沉淀法和溶劑熱法合成不同粒徑的磁性納米粒子,繼而將聚吡咯包覆在上述材料表面,結(jié)合磁性固相萃取-氣相色譜-質(zhì)譜檢測的方法,富集和檢測中藥樣品中四種擬除蟲菊酯類農(nóng)藥。將單因素實(shí)驗(yàn)用于優(yōu)化最佳萃取條件。在最優(yōu)條件下,線性相關(guān)系數(shù)R20.99,相對標(biāo)準(zhǔn)偏差(RSD)為2.6-3.8%,目標(biāo)物檢測限和定量限分別為0.016-0.064μgL-1和0.053-0.211μgL-1。將此方法用于市售中藥樣品中擬除蟲菊酯類農(nóng)藥的富集和檢測,獲得了滿意的結(jié)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，

本文編號：2482971