【作者】 卢鸯；

【导师】 朱岩；

【作者基本信息】 浙江大学 ， 化学， 2014， 博士

【摘要】 目前纺织品中有害物质检测中采用的样品前处理方法主要为传统的索氏提取、超声提取、液液萃取、旋转蒸发浓缩等。这些方法处理过程繁琐,所需时间长,而且通常需要消耗大量有机试剂,成本高,污染环境的同时也影响操作人员的身体健康。因此,发展快速、高效、简单、环保、经济、自动化程度高的样品前处理技术已成为业内共同关注的焦点。本论文正是基于以上考虑,将分散液液微萃取、加压热水萃取、溶剂诱导相变萃取等新型样品前处理方法应用于纺织品有害物质检测领域,以开发绿色、高效、快速、简单的检测新方法,在提高检测效率、降低检测成本和劳动强度的同时,提高方法的灵敏度和选择性。第一章简要介绍了目前纺织品中有害物质检测的现状和存在的问题；综述了分散液液微萃取、加压热水萃取、溶剂诱导相变萃取等新型样品前处理方法及其应用情况。第二章利用氯苯为萃取剂,乙腈为分散剂,以10种禁用芳香胺为代表,采用分散液液微萃取技术,快速萃取水相中的芳香胺,用气质联用法进行分析。实验考察了萃取剂的种类和体积、分散剂的种类和体积、萃取时间、盐效应等可能影响分散液液微萃取效率的因素。实验结果表明,与传统的液液萃取法相比,本方法具有操作简单、快速、准确、低成本及环境友好等优点,而且在抗基质干扰方面有更强的优势,检测灵敏度更高。第三章在第二章的基础上,建立了基于离子液体的旋涡辅助液液微萃取方法快速萃取水相中的芳香胺,用液相色谱进行分析。采用离子液体作为萃取剂,避免使用具有一定毒性和挥发性的卤代烃类有机溶剂,利用旋涡辅助混合手段代替分散剂的使用,方法更简单快速,更绿色环保。第四章首次将溶剂诱导相变萃取技术应用于纺织品中可分解芳香胺染料检测的前处理过程中,实验优化了诱导剂种类和体积、乙腈用量等影响萃取效率的参数。与现行标准方法相比,本方法具有操作简单、快速、对环境友好及基质干扰小等优点。第五章首次将加压热水萃取技术与旋涡辅助液液微萃取技术联用测定纺织品中氯苯类化合物。实验优化了萃取过程中的影响因素,并应用于实际样品检测中,与传统的索氏提取、超声提取方法做了比较。方法操作简单,选择性好,萃取时间短,且有机溶剂用量少,非常适应绿色化学发展的需要。第六章采用水为萃取剂,通过加速溶剂萃取,用水从纺织品/皮革样品中萃取富马酸二甲酯,再通过旋涡辅助液液微萃取方法对得到的水相萃取液中的待测物进行萃取、富集。建立了一种简单、高效、快速以及有机溶剂消耗少的测定纺织品/皮革样品中富马酸二甲酯的新方法。方法应用于实际样品的测定,取得了满意的结果。更多还原

【Abstract】 In currently accepted testing methods on pretreatment of textile samples, some conventional techniques such as Soxhlet extraction, ultrasonic extraction, liquid-liquid extraction were widely used. They are time-consuming and tedious. In addition, they always use a large volume of hazardous organic solvent and employ concentration procedures associated with the high risk of analyte losses. Nowadays, attention is focused on techniques that are rapid, simple, efficient, low-cost, and environmentally friendly by reduction or complete elimination of organic solvents.In this work, the applications of several types of novel sample pretreatment methods such as dispersive liquid-liquid microextraction (DLLME), pressurized hot water extraction (PHWE), solvent induced phase transition extraction (SIPTE) in potentially harmful substances testing for textiles were investigated. The aim of the study was to develop environmental-friendly, efficient, rapid and simple testing methods, not only reducing cost and labor intensity but increasing sensitivity and selectivity compared to existed methods.In Chapter one, the current situation and underlying questions of the conventional testing methods of harmful substances in textiles were pointed out. The chapter then focused on the introduction of several novel sample pretreatment methods such as dispersive liquid-liquid microextraction, vortex-assisted liquid-liquid microextraction, pressurized hot water extraction, accelerated solvent extraction, solvent induced phase transition extraction and their applications.In Chapter two, a dispersive liquid-liquid microextraction procedure coupled with gas chromatography-mass spectrometry was described for preconcentration and determination of10banned aromatic amines from textile samples. In this method, chlorobenzene and acetonitrile were used as extraction solvent and disperser solvent respectively. Experimental conditions affecting the microextraction procedure such as types and volumes of extraction solvent or disperser solvent, extraction time, salt concentration were optimized. Compared with the traditional liquid-liquid extraction, the proposed method demonstrated to be a simple, rapid, accurate, low-cost and environmentally friendly technique. In Chapter three, an ionic liquid-based vortex-assisted liquid-liquid microextraction coupled with high performance liquid chromatography was established to rapidly extract the aromatic amines in aqueous solution. Replacing toxic halogenated hydrocarbons with hydrophilic ionic liquid as extraction solvent was to avoid exposure danger to solvent for the operator. Moreover, the proposed method was faster, simpler, and more environment-friendly due to the dispersion of extraction organic solvent directly into the aqueous phase was achieved by vortex agitation rather than using disperser solvent.In Chapter four, for the first time, a simple extraction method termed solvent induced phase transition extraction was used for the analysis of banned aromatic amines in textile samples. The most favorable extraction variables in the extraction process were determined. The proposed method was much simpler and less time-consuming, it gave higher sensitivity, and used minimal amounts of organic solvents compared to previous existing methods.In Chapter five, the combination of pressurized hot water extraction with vortex-assisted liquid-liquid microextraction for sample preparation prior to gas chromatography-mass spectrometry analysis of chlorobenzenes in textiles was firstly reported here. Main factors potentially affecting the two extraction processes were evaluated and optimized. The developed method was then successfully used to analyze chlorobenzenes in real textile samples and was compared with the results from classical Soxhlet extraction and ultrasonic extraction. From the results obtained, the proposed method could be considered a reliable, low-cost approach and more environmentally friendly because it minimized the use of toxic organic solvents.In Chapter six, a simple, rapid, efficient and environmentally friendly sample preparation procedure coupled with gas chromatography-mass spectrometry was developed to assay dimethyl fumarate in textiles and leathers. The sample preparation procedure involved an accelerated solvent extraction using water as the extract solvent, followed by the extraction and concentration of dimethyl fumarate from the aqueous solution using vortex-assisted liquid-liquid microextraction. The developed method was successfully applied to textiles and leather samples.更多还原