混合半胶束磁性固相萃取和分散微固相萃取方法研究

发布时间：2018-04-15 20:49

本文选题：混合半胶束磁性固相萃取 + 分散微固相萃取　；参考：《河北大学》2016年硕士论文

【摘要】：作为一类重要的样品预处理方法,固相萃取已广泛应用于生物、食品和环境样品中目标化合物的萃取、净化和预浓缩。目前,固相萃取技术正向着小型化方向发展,出现了不同类型的小型化固相萃取方法,大大节省了人力和时间并减少了有机溶剂的使用。本论文主要对混合半胶束磁性固相萃取和分散微固相萃取这两种小型化固相萃取方法进行了研究,全文共分3章,其主要内容如下:第1章对固相萃取的研究现状及发展趋势进行了概述,重点介绍了固相微萃取、磁性固相萃取和分散微固相萃取,同时阐述了本文的选题思想。第2章利用CTAB包覆的Fe3O4混合半胶束磁性固相萃取结合HPLC-UV测定了饮用水中的四种合成雌激素。Fe3O4纳米粒子采用溶剂热法合成,并通过傅里叶变换红外光谱进行表征。实验考察了CTAB用量、水样p H值、Fe3O4用量、洗脱剂及水样体积对分析物萃取效率的影响,得出的最佳萃取条件为:20 mg CTAB;p H为11;100 mg Fe3O4;洗脱剂为3 m L含1%HAc的乙腈;水样体积为300 m L。双酚A、己烯雌酚、辛基酚和壬基酚的线性关系良好(R20.9996),四种物质的LOD在0.011-0.037μg/m L之间。在最佳条件下,分别检测了两种饮用水中四种合成雌激素的含量,加标回收率在75.8%-106.0%之间。方法的日内精密度和日间精密度的RSD值分别小于4.31%和5.70%。本文结合了混合半胶束和磁性纳米离子的优点,磁性分离简化了分离操作,CTAB作为萃取介质减少了有机溶剂的使用,对环境友好。第3章利用壳聚糖辅助针管内分散微固相萃取结合HPLC-UV测定了三种含大黄口服液中的三种蒽醌类物质。实验考察了壳聚糖浓度、壳聚糖种类、萃取时间、p H值、洗脱剂种类和体积对大黄素、大黄酚和大黄素甲醚萃取效率的影响,得出的最佳萃取条件为:壳聚糖浓度为0.6μg/m L、分子量为3000、萃取时间为2 min、p H值为5、洗脱剂为800μL甲醇。在最佳萃取条件下,三种蒽醌类物质呈现出良好的线性关系,线性范围在5-100 ng/m L之间,线性相关系数R20.998;三种物质的检出限在1.8-3.0 ng/m L范围内;方法的日间精密度和日内精密度的RSD值分别小于4.68%和5.36%。将此方法成功应用于黄栀花口服液、儿童清热口服液和厚朴排气合剂中三种蒽醌类物质含量的测定,三种口服液中的大黄素含量在28.4-64.3 ng/m L之间、大黄酚含量在42.7-57.0 ng/m L之间、大黄素甲醚含量在8.1-10.7 ng/m L之间,三种蒽醌类物质的样品加标回收率在85.9%-120.3%之间。本实验第一次使用壳聚糖分散微固相萃取结合高效液相色谱-紫外检测法测定了口服液中蒽醌类物质,实验结果令人满意。
[Abstract]:As an important sample pretreatment method, solid phase extraction (SPE) has been widely used in the extraction, purification and preconcentration of target compounds in biological, food and environmental samples.At present, solid phase extraction (SPE) technology is developing towards miniaturization. Different kinds of miniaturization solid-phase extraction (SPE) methods have emerged, which have greatly saved manpower and time and reduced the use of organic solvents.In this paper, two miniaturized solid phase extraction methods, mixed semi-micellar magnetic solid phase extraction and dispersed microsolid phase extraction, are studied.The main contents are as follows: in Chapter 1, the research status and development trend of SPE are summarized, with emphasis on solid-phase microextraction (SPME), magnetic solid-phase extraction (SPE) and dispersed microsolid-phase extraction (DESPE).In chapter 2, four synthetic estrogens. Fe _ 3O _ 4 nanoparticles in drinking water were synthesized by solvothermal method and characterized by Fourier transform infrared spectroscopy (FTIR) using CTAB coated Fe3O4 mixed semi-micelle magnetic solid phase extraction (SPE) combined with HPLC-UV.The effects of CTAB dosage, pH value of water sample, amount of Fe 3O 4, eluent and volume of water sample on the extraction efficiency of the analyte were investigated. The optimum extraction conditions were obtained as follows: 1: 20 mg CTABX H = 11100 mg Fe 3O 4, 3 mL acetonitrile containing 1%HAc, and 300 mL water sample volume.The linear relationship between bisphenol A, diethylstilbestrol, octylphenol and nonylphenol is good. The LOD of the four compounds is 0.011-0.037 渭 g / mL.Under the optimum conditions, the contents of four synthetic estrogens in two kinds of drinking water were determined, and the recoveries were between 75.8- 106.0%.The RSD values of intra-day precision and inter-day precision were less than 4.31% and 5.70%, respectively.In this paper, the advantages of mixed semi-micelles and magnetic nanoscale ions are combined. Magnetic separation simplifies the separation operation of CTAB as an extraction medium and reduces the use of organic solvents and is environmentally friendly.In chapter 3, three anthraquinones in rhubarb oral liquid were determined by chitosan assisted microsolid phase extraction and HPLC-UV.The effects of concentration of chitosan, kinds of chitosan, extraction time and pH value, kinds and volume of eluent on the extraction efficiency of emodin, chrysophanol and emodin methyl ether were investigated.The optimum extraction conditions are as follows: chitosan concentration is 0.6 渭 g / mL, molecular weight is 3000, extraction time is 2 min, pH value is 5, eluent is 800 渭 L methanol.Under the optimum extraction conditions, the three anthraquinones showed a good linear relationship, with a linear range of 5-100 ng/m / L and a linear correlation coefficient R20.998.The detection limits of the three compounds were in the range of 1.8-3.0 ng/m / L.The RSD values of day precision and intra-day precision were less than 4.68% and 5.36%, respectively.The method was successfully applied to the determination of three anthraquinones in Huangzhihua oral liquid, children's Qingre oral liquid and Houpu exhaust mixture. The emodin content in the three oral liquids ranged from 28.4-64.3 ng/m / L, and the chrysophanol content was 42.7-57.0 ng/m / L.The content of emodin methyl ether ranged from 8.1 to 10.7 ng/m / L, and the recoveries of the three anthraquinones were between 85.9- 120.3%.The anthraquinones in oral liquid were determined by chitosan dispersive microsolid phase extraction and high performance liquid chromatography-ultraviolet detection for the first time. The experimental results were satisfactory.
【学位授予单位】：河北大学
【学位级别】：硕士
【学位授予年份】：2016
【分类号】：O658.2

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