新型样品前处理技术在有机污染物分析中的应用研究

发布时间：2018-06-09 21:48

本文选题：样品前处理 + 液相微萃取　；参考：《中国农业大学》2015年博士论文

【摘要】：样品前处理是农药残留分析中最重要的环节,开发高效、环保的样品前处理技术变得越来越重要。液相微萃取技术(liquid-phase microextraction, LPME)微固相萃取技术(micro-solid phase extraction, μ-SPE)是近些年出现的新型样品前处理技术。这两种新型的样品前处理技术集萃取、净化、浓缩、进样于一体,在保证萃取效率的同时,有效的缩短了萃取时间。与传统方法比这两种方法更加简单、快速和对环境友好。本论文在前人已有研究的基础上,以样品前处理方法中的液相微萃取技术和微固相萃取技术为研究方向,主要开发了三种新型的液相微萃取技术和一种微固相萃取技术,并成功应用于食品和环境样本中目标分析物的检测。这4种方法都是针对日前新型的样品前处理技术发展中存在的缺点和遇到的瓶颈问题进行改进和创新。具体内容如下：建立了一种可以轻松分离轻溶剂和样品溶液的分散液液微萃取的方法,并与气相色谱-电子捕获检测器联用；提出用轻溶剂分散液液微萃取(low density solvent based dispersive liquid-liquid microextraction, LDS-DLLME)的方法检测雪水中的17种有机氯农药残留,该方法回收率大于71.4%,检出限在0.02-0.11μg/L之间,相对标准偏差范围在1.6%-14.8%之间。该方法克服了轻溶剂需要使用特殊容器、操作繁琐等缺点,成为了一种简便、快速、环境友好的前处理技术。建立了一种使用轻溶剂的超声辅助液相微萃取(USA-LPME)方法检测土壤样品中的9种有机氯农药残留,方法的回收率大于71.6%,检出限为0.04-0.18μg/kg,相对标准偏差在6.7%-19.6%之间。该方法实现了液相微萃取技术在固体复杂基质中的应用,操作简便、萃取时间短、效率高、对环境友好。建立了一种超分子溶剂微萃取(SUSME)方法检测啤酒中的手性杀菌剂三唑峒和三唑醇的残留,检测仪器为高效液相色谱串联三重四极杆质谱(HPLC-MS/MS),并在相同条件下与传统有机溶剂进行对比,超分子溶剂的萃取能力明显好于其它有机溶剂。该方法回收率大于84%,检出限为0.24-0.98μg/L,相对标准偏差为1.6%-5.7%。开发了氮吹辅助微固相萃取(NFA-μSPE)方法检测环境水样本中挥发性的有机污染物,该方法以活性炭作为吸附剂,并借助过滤器制作了一种新型的萃取装置与气相色谱串联三重四极杆质谱(GC-MS/MS)联用。该方法的回收率大于77.9%,检出限在0.008-0.023μg/L之间,相对标准偏差在6.9%-10.4%之间。所有建立与开发的方法都是省时省力,环境友好的样品前处理技术,并目.通过优化实验,将新方法成功的应用于实际样品的分析检测中,而且都得到了较好的萃取结果。
[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.
【学位授予单位】：中国农业大学
【学位级别】：博士
【学位授予年份】：2015
【分类号】：S481.8

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