痕量有机污染物的微萃取及分析应用研究

发布时间：2018-04-10 16:33

  本文选题：离子液体分散液液微萃取尿样 + 3-羟基苯并[a]芘　； 参考：《中国科学技术大学》2016年硕士论文

【摘要】：随着分析技术的发展,样品前处理技术朝着高效、快速、绿色、自动化与微型化的方向发展。本论文综述了几种常见的基于相分配及相吸附原理的样品前处理技术,分别介绍了它们的原理、特点及应用。在充分调研文献的基础上,本论文主要进行了以下几部分的研究工作：1.建立了离子液体-分散液液微萃取／高效液相色谱-荧光检测法测定吸烟人群尿样中3-羟基苯并[a]芘的分析方法。尿样经酶解、滤膜过滤后,采用[C8MIM][PF6]为萃取剂进行分散液液微萃取富集,移取沉积相进行液相色谱分析。实验对酶解条件、萃取条件及荧光测量条件进行了优化。在最佳的实验条件下,方法在1.5-150ng/L浓度范围内具备良好的线性关系(r20.996),富集倍数约为180。检出限(LOD)和测定下限(LOQ)分别为0.45和1.5 ng/L。加标回收率为85.6-94.6%,相对标准偏差(RSD)为3.4-5.2%。2.建立了离子液体-分散液液微萃取-丹磺酰氯衍生／高效液相色谱串联质谱法测定尿样中3-羟基苯并[a]芘的分析方法。尿样经酶解、滤膜过滤、采用[C8MIM][PF6]为萃取剂进行分散液液微萃取富集后,采用丹磺酰氯作为衍生试剂对3-OHBaP进行化学衍生,移取沉积相进行液相色谱串联质谱分析。实验对丹磺酰氯衍生条件进行了优化。在最佳的实验条件下,方法在0.6~50.0 ng/L浓度范围内具备良好的线性关系(r2≥0.9918)。LOD与LOQ分别为0.2和0.58 ng/L。加标回收率为87.8%～96.2%,RSD为3.3%~6.8%。3.在分散液液微萃取与磁性固相萃取的基础上,研究了一种新型的分散固液微萃取技术。建立了磁性分散固液微萃取-在线热解析-气质联用法测定烟叶中易挥发的中性香气成分的分析方法。本文自制了CIP-SiO2-PDMS磁性吸附剂,通过红外、热重、透射电镜、扫描电镜等方法对材料进行了表征。实验对CIP-SiO2-PDMS磁性吸附剂的合成条件、萃取条件和解析条件进行了优化。最后采用本方法对若干种挥发性中性香气成分进行了分析。
[Abstract]:With the development of analytical technology, sample pretreatment technology develops towards high efficiency, fast, green, automation and miniaturization.In this paper, several common sample pretreatment techniques based on phase distribution and phase adsorption are reviewed, and their principles, characteristics and applications are introduced respectively.On the basis of full investigation and research, this paper mainly carried out the following parts of the research work: 1.A method for the determination of 3-hydroxybenzo [a] pyrene in urine samples of smoking population by ion liquid-dispersible liquid microextraction / high performance liquid chromatography-fluorescence detection was established.Urine samples were hydrolyzed by enzyme and filtrated by filter membrane, then [C8MIM] [PF6] was used as extractant for dispersible liquid microextraction enrichment, and the deposition phase was removed for liquid chromatographic analysis.The conditions of enzymatic hydrolysis, extraction and fluorescence measurement were optimized.Under the optimum experimental conditions, the method has a good linear relationship in the concentration range of 1.5-150ng/L, r20.996, and the enrichment factor is about 180.The detection limit (LOD) and the determination limit (LOQ) were 0.45 and 1.5 ng / L, respectively.The recoveries were 85.6-94.6 and the relative standard deviation (RSDs) was 3.4-5.2. 2.A method for the determination of 3-hydroxybenzo [a] pyrene in urine by ion liquid-dispersible liquid microextraction with dansulfoyl chloride derivation / high performance liquid chromatography tandem mass spectrometry was established.Urine samples were hydrolyzed by enzyme, filtrated by filter membrane, and enriched with [C8MIM] [PF6] as extractant. After microextraction and enrichment with [C8MIM] [PF6] as extractant, the 3-OHBaP was chemically derivated by dansulfoyl chloride, and the deposition phase was removed and analyzed by liquid chromatography tandem mass spectrometry (LC-MS).The derivatization conditions of dansulfonyl chloride were optimized.Under the optimum experimental conditions, the linear relationship between 0.9918).LOD 鈮，

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