悬浮固化分散液相微萃取技术测定水样中环境激素的研究

发布时间：2018-06-22 17:24

本文选题：悬浮固化分散液相微萃取 + 高效液相色谱串联质谱　；参考：《苏州科技大学》2017年硕士论文

【摘要】：悬浮固化分散液相微萃取(Dispersive Liquid-Liquid MicroextractionSolidification of Floating Organic Drop,简称DLLME-SFO)是21世纪初期提出的一种样品前处理的新方法,该法运用密度比水小、熔点接近室温的萃取剂,在微波辅助下形成水、萃取剂和分散剂的三元混合乳浊液。该法操作简单、萃取快速高效,因而在环境、食品、医药等方面具有广泛应用。本论文的主要内容如下:第一章介绍了目前较为普遍使用的样品前处理方法,着重介绍悬浮固化分散液相微萃取(DLLME-SFO)技术的发展过程、原理以及操作步骤,在分析领域中的应用以及改进。第二章建立了悬浮固化分散液相微萃取(DLLME-SFO)联用高效液相色谱(HPLC)串联质谱(MS/MS)法测定水样中的6种雌激素的分析方法。萃取的最优条件为:调节水样pH为7,以90μL 1-十二醇为萃取剂,250μL Tritonx-100(0.025mol/L)为分散剂,在25°C下,超声3 min,对雌激素进行萃取。最优条件下,该方法在三个浓度水平下的平均加标回收率为93.4%-108.6%,相对标准偏差为1.3%-8.7%,方法的检出限为0.001-0.05μg/L。将该方法应用于检测水样品中雌激素残留,获得了令人满意的结果。第三章建立了悬浮固化分散液相微萃取(DLLME-SFO)联用气相色谱(GC)串联质谱法(MS/MS)分析检测环境水样品中残留的15种邻苯二甲酸酯(PAEs)的检测方法。通过各影响因素对比试验,得出最佳萃取条件及所用仪器的最佳色谱和质谱条件。在最优条件下,高、低两个浓度水平下平均加标回收率为72.0%-122.0%,相对标准偏差为0.4%-8.0%,方法的检出限为0.022-0.149μg/L。结果表明,该方法被成功的应用于测定水样中邻苯二甲酸酯类污染物。
[Abstract]:Dispersive Liquid-Liquid MicroextractionSolidification of floating Organic Dropp (DLLME-SFO) is a new method of sample pretreatment proposed in the early 21st century. Ternary emulsion of extractant and dispersant. Because of its simple operation and rapid extraction, this method is widely used in environment, food, medicine and so on. The main contents of this thesis are as follows: in the first chapter, the popular sample pretreatment methods are introduced, and the development process, principle and operation steps of suspension solidified dispersed liquid phase microextraction (DLLME-SFO) technology are emphatically introduced. Application and improvement in the field of analysis. In chapter 2, a method for the determination of six estrogens in water samples by suspension solidified dispersed liquid phase microextraction (DLLME-SFO) and high performance liquid chromatography (HPLC) tandem mass spectrometry (MS / MS) was established. The optimum extraction conditions were as follows: adjusting the pH of water sample to 7, using 90 渭 L 1-dodecanol as extractant and 250 渭 L Tritonx-100 (0.025 mol / L) as dispersant, at 25 掳C, ultrasound for 3 min to extract estrogen. Under the optimum conditions, the average recoveries of the method were 93.4- 108.6, the relative standard deviation was 1.3- 8.7.The detection limit of the method was 0.001-0.05 渭 g 路L ~ (-1) 路L ~ (-1) 路L ~ (-1) 路L ~ (-1) 路L ~ (-1) 路L ~ (-1) 路L ~ (-1) ~ (-1) ~ (-1). The method has been applied to the determination of estrogen residues in water samples with satisfactory results. In chapter 3, a method for the determination of 15 kinds of phthalates (PAEs) in environmental water samples by suspension solidified dispersed liquid phase microextraction (DLLME-SFO) and gas chromatography (GC) tandem mass spectrometry (MS / MS) was established. The optimum extraction conditions and the optimum conditions of chromatography-mass spectrometry for the instruments used were obtained through the comparative tests of various influencing factors. Under the optimum conditions, the average recoveries were 72.0-122.0, the relative standard deviations were 0.4- 8.0, and the detection limits were 0.022-0.149 渭 g / L at high and low concentrations. The results show that the method has been successfully applied to the determination of phthalic acid esters in water samples.
【学位授予单位】：苏州科技大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：X832

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