新型样品前处理技术在环境和生物样品分析中的应用

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英文题名：Application of New Sample Preparation Technique to the Analysis of Environmental and Biological Samples 作者：胡西洲 论文级别：博士 学科专业名称：分析化学 中文关键词：样品前处理 ; 固相微萃取 ; 液相微萃取 ; 环境分析 ; 生物分析 英文关键词：sample preparation technique ; solid phase microextraction ; liquid phase microextraction ; environmental analysis ; biological analysis 学位年度：2012 导师：冯钰锜 学科代码：070302 学位授予单位：武汉大学 论文提交日期：2012-05-01

摘要

近年来，微型化样品制备技术越来越受到分析工作者的青睐，一些微型化、无需或仅需使用少量溶剂的样品制备技术得到了迅速的发展，如固相微萃取和液相微萃取。这两种技术克服了传统的样品制备过程中出现的繁琐操作、耗时、消耗大量的样品及有机溶剂等诸多不足，以简便、灵活、易操作、环境友好等特征顺应分析化学发展的要求，通过与各种分析仪器的联用，能有效地应用到多种样品中分析物的分离和富集。随着新型萃取介质和萃取模式、高通量及自动化萃取装置的不断发展，微萃取技术在食品、环境、生物及医药分析等众多分析领域中将发挥越来越重要的作用。
     本论文围绕新型固相微萃取和液相微萃取技术在环境和生物样品分析中的应用开展了一些工作，主要研究内容如下：
     1．介绍了样品前处理技术的发展概况，并从基本理论、萃取模式、影响萃取效率的因素、实际应用及其进展等几个方面分别对固相微萃取和液相微萃取技术进行了全面的综述。
     2．将聚合物整体柱固相微萃取技术与高效液相色谱-质谱联用，建立了在鸡蛋、牛奶、鸡肉和猪肉中苯并咪唑类药物的多残留检测方法。以聚甲基丙烯酸-乙二醇二甲基丙烯酸酯整体柱为萃取材料，在优化的实验条件下，该材料对分析物具有很强的萃取能力，在随后的分析中没有发现杂质峰对定量的影响。最后，该方法成功应用于口饲阿苯达唑的母鸡所产鸡蛋中的阿苯达唑及其代谢物的测定。
     3．以Fe3O4/SiO2/Poly (MAA-co-EDMA)磁性复合材料为萃取介质，构建了磁固相萃取-毛细管电泳联用方法，结合场放大样品堆积技术，实现了对猪组织样品中10种苯并咪唑类药物的快速分析。结果表明，该方法线性关系良好，且具有较好的精密度和准确度。磁固相萃取与毛细管电泳的结合将为兽药多残留检测提供新的实用工具。
     4．建立了一种基于分子络合物-分散液液微萃取技术及其对水溶液中酚类化合物的快速检测方法。与常规分散液液微萃取使用的有机溶剂不同的是，该方法以磷酸三丁酯（路易斯碱）作为萃取剂，与水溶液中酚类化合物（路易斯酸）通过路易斯酸碱作用取得满意的萃取效果。此外，萃取是在廉价的一次性滴管中完成，在滴管细的颈部很方便地收集低密度的萃取剂。该方法的建立为分散液液微萃取应用于极性化合物的萃取提供新的思路。
     5．将固相萃取与分子络合物-分散液液微萃取相结合与高效液相色谱联用，建立了一种测定椰子汁中酸性植物激素的新方法。选择吲哚乙酸、水杨酸、脱落酸和吲哚丁酸为分析物并考察了其萃取性能。在固相萃取与分子络合物-分散液液微萃取联用模式中，椰子汁中分析物首先吸附在C18萃取材料上，解吸完成后，解吸液又可用作分散液液微萃取的分散剂。该方法的富集倍数可达319.1-477.7倍，该方法线性关系良好，且具有良好的精密度和准确度。
Nowadays, more favour has been focused on miniaturated sample preparationtechnique, and some miniaturated, less solvent or solvent-free sample preparationtechnique, such as solid phase microextraction and liquid phase microextraction, havebeen developed rapidly, which conquers some shortcomings of labourious operation,time-consuming, high consumption of sample and reagent, etc. Being possessadvantages including simple, flexible, easily operational, environmental friendly, thetwo extraction techniques meet the development trend in practical application coulpedwith all kinds analytical instruments. With the unceasing development of new extractionmaterials, modes, high throughout, and automated devices in sample preparationtechnique, microextraction technique will play more important role in food,environmental, biological and medical analysis.
     In this dissertation, some applications were developed through two newmicroextrction techniques in environmental and biological analysis. These workinvolved are list below:
     1. The development of sample preparation was introduced, and foundation,extraction modes, influencing factors, the applications and developments of solid phasemicroextraction and liquid phase microextraction were reviewed comprehensively.
     2. A sensitive method has been established for the simultaneous analysis ofbenzimidazole multi-residues in egg, milk, chicken, and pork. This method is based onthe combination of polymer monolith microextraction (PMME) technique with liquidchromatography and electrospray ionization mass spectrometry (LC-ESI/MS). Theextraction was performed with a poly (methacrylic acid-co-ethylene glycoldimethacrylate)(MAA-co-EGDMA) monolithic capillary column. Under the optimizedextraction conditions, good extraction efficiencies for the targets were obtained, and nointerferences from the matrix were observed for the quantification of the analytes in thesubsequent detection. The method was later successfully applied for the determinationof primary and metabolite residues in eggs after oral administration of albendazole tohens.
     3. A simple, rapid, and efficient method for simultaneous determination of tenbenzimidazole drugs in animal tissues samples was developed. This analyticalprocedure involved extracting samples with magnetic solid-phase extraction (MSPE)using magnetite/silica/poly (methacrylic acid-co-ethylene glycol dimethacrylate)(Fe3O4/SiO2/Poly (MAA-co-EGDMA)) magnetic microspheres, and determination bycapillary electrophoresis (CE) with field-amplified sample stacking technique (FASS).The results showed good linearities were obtained for the analytes, and the developedmethod has also good precision and accuracy. The combination of MSPE and CE willpovide new practical tool for veterinary drug multi-residues analysis.
     4. A novel molecular complex-based dispersive liquid-liquid microextraction(DLLME) method was established and applied to fast analysis of phenols in aqueoussolution. In this approach, tri-n-butylphosphate (TBP), a Lewis base, was directly used,instead of the traditional water-immiscible organic solvents, as the extractant forDLLME. The phenols, which are typical Lewis acids, were successfully extracted fromaqueous samples. In addition, extraction was accomplished in a disposable polyethylenepipet with the open and narrow tip upside, for an easy collection of the above extractantlayer, i.e. TBP. The developed approach provides a new way to facilitate DLLME oforganic polar compounds from aqueous solutions.
     5. A new method combined the solid-phase extraction (SPE) and the molecularcomplex-based dispersive liquid-liquid microextraction (MC-DLLME) has beendeveloped for the determination of several acidic phytohormones in natural coconutjuice. Indole-3-acetic acid (IAA), salicylic acid (SA), abscisic acid (ABA) andindolyl-3-butyricacid (IBA) were selected to assess the extraction procedure anddetermined by liquid chromatography with ultraviolet detection (LC-UV). Insolid-phase extraction-dispersive liquid-liquid microextraction (SPE-DLLME), analyteswere firstly adsorbed into C18sorbent from a large volume of coconut juice samples.The eluate containing the desired compounds was outflowed from the sorbent by usingmethanol, which was used as the dispersive solvent in MC-DLLME procedure. The newmethod provided a high enrichment factor (319.1-477.7) for several acidicphytohormones. Good linearities were obtained for the analytes, and the developed method has also good precision and accuracy.

引文

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