發(fā)布時間：2018-06-09 21:48

  本文選題：樣品前處理 + 液相微萃取��； 參考：《中國農(nóng)業(yè)大學》2015年博士論文

【摘要】：樣品前處理是農(nóng)藥殘留分析中最重要的環(huán)節(jié),開發(fā)高效、環(huán)保的樣品前處理技術變得越來越重要。液相微萃取技術(liquid-phase microextraction, LPME)微固相萃取技術(micro-solid phase extraction, μ-SPE)是近些年出現(xiàn)的新型樣品前處理技術。這兩種新型的樣品前處理技術集萃取、凈化、濃縮、進樣于一體,在保證萃取效率的同時,有效的縮短了萃取時間。與傳統(tǒng)方法比這兩種方法更加簡單、快速和對環(huán)境友好。本論文在前人已有研究的基礎上,以樣品前處理方法中的液相微萃取技術和微固相萃取技術為研究方向,主要開發(fā)了三種新型的液相微萃取技術和一種微固相萃取技術,并成功應用于食品和環(huán)境樣本中目標分析物的檢測。這4種方法都是針對日前新型的樣品前處理技術發(fā)展中存在的缺點和遇到的瓶頸問題進行改進和創(chuàng)新。具體內(nèi)容如下： 建立了一種可以輕松分離輕溶劑和樣品溶液的分散液液微萃取的方法,并與氣相色譜-電子捕獲檢測器聯(lián)用；提出用輕溶劑分散液液微萃取(low density solvent based dispersive liquid-liquid microextraction, LDS-DLLME)的方法檢測雪水中的17種有機氯農(nóng)藥殘留,該方法回收率大于71.4%,檢出限在0.02-0.11μg/L之間,相對標準偏差范圍在1.6%-14.8%之間。該方法克服了輕溶劑需要使用特殊容器、操作繁瑣等缺點,成為了一種簡便、快速、環(huán)境友好的前處理技術。 建立了一種使用輕溶劑的超聲輔助液相微萃取(USA-LPME)方法檢測土壤樣品中的9種有機氯農(nóng)藥殘留,方法的回收率大于71.6%,檢出限為0.04-0.18μg/kg,相對標準偏差在6.7%-19.6%之間。該方法實現(xiàn)了液相微萃取技術在固體復雜基質中的應用,操作簡便、萃取時間短、效率高、對環(huán)境友好。 建立了一種超分子溶劑微萃取(SUSME)方法檢測啤酒中的手性殺菌劑三唑峒和三唑醇的殘留,檢測儀器為高效液相色譜串聯(lián)三重四極桿質譜(HPLC-MS/MS),并在相同條件下與傳統(tǒng)有機溶劑進行對比,超分子溶劑的萃取能力明顯好于其它有機溶劑。該方法回收率大于84%,檢出限為0.24-0.98μg/L,相對標準偏差為1.6%-5.7%。 開發(fā)了氮吹輔助微固相萃取(NFA-μSPE)方法檢測環(huán)境水樣本中揮發(fā)性的有機污染物,該方法以活性炭作為吸附劑,并借助過濾器制作了一種新型的萃取裝置與氣相色譜串聯(lián)三重四極桿質譜(GC-MS/MS)聯(lián)用。該方法的回收率大于77.9%,檢出限在0.008-0.023μg/L之間,相對標準偏差在6.9%-10.4%之間。 所有建立與開發(fā)的方法都是省時省力,環(huán)境友好的樣品前處理技術,并目.通過優(yōu)化實驗,將新方法成功的應用于實際樣品的分析檢測中,而且都得到了較好的萃取結果。
[Abstract]:Sample pretreatment is the most important part in pesticide residue analysis. It is becoming more and more important to develop efficient and environmentally friendly sample pretreatment technology. Liquid-phase microextraction (LPME) micro-solid phase extraction (渭 -SPE) is a new sample pretreatment technology in recent years. These two new sample pretreatment techniques are integrated with extraction, purification, concentration and sample injection, which can effectively shorten the extraction time while ensuring the extraction efficiency. These two methods are simpler, faster and more environmentally friendly than traditional methods. On the basis of previous studies, three new liquid phase microextraction techniques and one microsolid phase extraction technology are developed in this paper, which are mainly based on liquid phase microextraction and microsolid phase extraction. It has been successfully applied to the detection of target analytes in food and environmental samples. These four methods are aimed at improving and innovating the shortcomings and bottlenecks encountered in the development of the new sample pretreatment technology. The main contents are as follows: a method for the easy separation of light solvent and sample solution by dispersive liquid microextraction was established and was combined with gas chromatography-electron capture detector (GC). A method for the determination of 17 organochlorine pesticide residues in snow water with low density solvent based dispersive liquid-liquid microextraction (LDS-DLLME) was proposed. The recovery rate of the method was greater than 71.4 and the detection limit was between 0.02-0.11 渭 g / L, and the relative standard deviation was between 1.6 and 14.8%. This method overcomes the disadvantages of using special container and complicated operation in light solvent, so it becomes a simple and fast method. An environmentally friendly pretreatment technique was developed for the determination of 9 organochlorine pesticide residues in soil samples by ultrasonic assisted liquid phase microextraction (USA-LPME-US) with a detection limit of 0.04-0.18 渭 g / kg. The relative standard deviation was between 6.7% and 19.6%. This method has realized the application of liquid phase microextraction technology in solid complex matrix, which is easy to operate, short in extraction time and high in efficiency. A supramolecular solvent microextraction (SUSME) method was developed for the determination of the residues of chiral fungicides triazolone and triazolol in beer. High performance liquid chromatography (HPLC) series triple quadrupole mass spectrometry (HPLC-MS / MS / MS) was used to detect HPLC-MS / MS, and compared with traditional organic solvents under the same conditions, the extraction ability of supramolecular solvents was obviously better than that of other organic solvents. The recovery rate of this method is greater than 84g / L, the detection limit is 0.24-0.98 渭 g / L, and the relative standard deviation is 1.6-5.7.The nitrogen blowing assisted microsolid phase extraction (NFA- 渭 SPE) method for the determination of volatile organic pollutants in environmental water samples is developed. The activated carbon is used as adsorbent for the determination of volatile organic pollutants in environmental water samples. A new type of extraction device and gas chromatography tandem triple quadrupole mass spectrometry (GC-MS / MS) was developed with the help of filter. The recovery rate of this method is greater than 77.9 渭 g / L, the detection limit is 0.008-0.023 渭 g / L, and the relative standard deviation is 6.9- 10.4%. All the methods established and developed are time-saving and environmentally friendly sample pretreatment techniques. Through the optimization experiment, the new method is successfully applied to the analysis and detection of practical samples, and good extraction results are obtained.
【學位授予單位】：中國農(nóng)業(yè)大學
【學位級別】：博士
【學位授予年份】：2015
【分類號】：S481.8

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本文編號：2000945