農(nóng)產(chǎn)品中阿特拉津殘留的快速、高靈敏SPR檢測(cè)方法研究
本文選題:表面等離子共振(SPR) + 金納米粒子。 參考:《湖南農(nóng)業(yè)大學(xué)》2012年碩士論文
【摘要】:阿特拉津是目前世界上使用范圍最廣、使用量最大的一種旱田除草劑,其化學(xué)性質(zhì)比較穩(wěn)定,在自然環(huán)境中不易被分解,能夠長(zhǎng)期存留在土壤和水中,污染自然環(huán)境;農(nóng)作物的根系及莖中也會(huì)有殘留,危害人體健康。因此,對(duì)阿特拉津的檢測(cè)與監(jiān)控就變得十分必要。目前,有多種阿特拉津檢測(cè)方法,但這些方法都不同程度地存在著操作復(fù)雜、耗時(shí)長(zhǎng)、樣品前處理復(fù)雜等缺點(diǎn),探索新的阿特拉津檢測(cè)方法變得越來(lái)越重要。表面等離子共振(surface plasmon resonance, SPR)技術(shù)具有高靈敏度,操作簡(jiǎn)單,檢測(cè)時(shí)間短,無(wú)須標(biāo)記,耗樣量少,能實(shí)時(shí)監(jiān)測(cè)反應(yīng)動(dòng)態(tài)過(guò)程,只需對(duì)樣品進(jìn)行簡(jiǎn)單的前處理,也可無(wú)須純化各種生物組分等優(yōu)點(diǎn),已經(jīng)被國(guó)內(nèi)外各實(shí)驗(yàn)室廣泛應(yīng)用于多個(gè)研究領(lǐng)域。該技術(shù)不但可檢測(cè)分析物,而且可測(cè)定分子之間相互作用的動(dòng)力學(xué)常數(shù)。目前,SPR在檢測(cè)阿特拉津殘留方面做了大量的研究工作,但是對(duì)實(shí)際樣品的檢測(cè)僅以自然界的水源為主,農(nóng)產(chǎn)品實(shí)際樣品的檢測(cè)和加標(biāo)回收率很少涉及。 本文研究并建立了四種SPR檢測(cè)除草劑阿特拉津的新方法,分別是:利用氨基團(tuán)置換阿特拉津的氯基團(tuán),SPR競(jìng)爭(zhēng)檢測(cè)阿特拉津(改良競(jìng)爭(zhēng)法);利用金納米粒子增強(qiáng)SPR靈敏度直接檢測(cè)阿特拉津;利用磁納米粒子增強(qiáng)SPR靈敏度直接檢測(cè)阿特拉津;利用磁納米粒子增強(qiáng)SPR靈敏度,結(jié)合改良競(jìng)爭(zhēng)法檢測(cè)阿特拉津。上述四種方法的最低檢測(cè)濃度依次為:10pg/mL、2pg/ml、2pg/mL和0.5pg/mL。同時(shí)利用上述四種方法對(duì)農(nóng)產(chǎn)品中阿特拉津使用量較大的甘蔗和玉米進(jìn)行實(shí)際樣品的檢測(cè),并運(yùn)用加標(biāo)回收率試驗(yàn)分別驗(yàn)證上述所建立的四種新方法的準(zhǔn)確度和重現(xiàn)性。實(shí)驗(yàn)結(jié)果表明,本文建立的四種方法都具有很低的最低檢測(cè)濃度,回收率試驗(yàn)也均呈現(xiàn)出較好的準(zhǔn)確性和重現(xiàn)性。文中最后對(duì)SPR傳感芯片的再生方法進(jìn)行研究,研究結(jié)果表明酒精-水虎魚(yú)綜合再生處理SPR舊金片的效果最好。
[Abstract]:Atrazine is one of the most widely used and used herbicides in the world at present. Its chemical properties are stable and it is difficult to be decomposed in the natural environment. It can be kept in soil and water for a long time and pollute the natural environment.There are also residues in the roots and stems of crops, endangering human health.Therefore, the detection and monitoring of atrazine become very necessary.At present, there are a variety of atrazine detection methods, but to varying degrees, these methods have the disadvantages of complex operation, long time consumption and complex sample pretreatment, so it is becoming more and more important to explore new methods for the detection of atrazine.The surface plasmon resonance (SPR) technique has the advantages of high sensitivity, simple operation, short detection time, no marking, less sample consumption, real-time monitoring of the dynamic process of reaction, and simple pretreatment of the sample.It has been widely used in many research fields at home and abroad.This technique can not only detect analytes, but also determine the kinetic constants of molecular interactions.At present, a great deal of research work has been done on the detection of atrazine residues by SPR, but the detection of real samples is mainly based on the source of water in nature, and the detection and standard recovery of agricultural products are seldom involved.In this paper, four new SPR methods for the detection of herbicide atrazine were studied and established.The results showed that atrazine was detected by using amino groups to replace atrazine (modified competition law), gold nanoparticles were used to enhance the sensitivity of SPR to detect atrazine directly.Atrazine was directly detected by magnetic nanoparticles enhanced SPR sensitivity, and atrazine was detected by magnetic nanoparticles enhanced SPR sensitivity combined with improved competition law.The lowest detection concentrations of the above four methods were: 1 10 PG / mL 2 PG / ml 2 PG / mL and 0.5 PG / mL respectively.At the same time, the above four methods were used to detect the actual samples of sugarcane and corn with large amount of atrazine in agricultural products, and the accuracy and reproducibility of the four new methods were verified by the standard adding recovery test.The experimental results show that the four methods developed in this paper have very low detection concentration, and the recovery test also shows good accuracy and reproducibility.Finally, the regeneration method of SPR sensor chip was studied. The results showed that the comprehensive regeneration of SPR was the best.
【學(xué)位授予單位】:湖南農(nóng)業(yè)大學(xué)
【學(xué)位級(jí)別】:碩士
【學(xué)位授予年份】:2012
【分類號(hào)】:R155.5
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