固相萃取新技术与痕量金属分离富集及形态分析研究
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摘要
人类的社会和科技活动造成了严重的环境污染,其中金属元素污染已经成为一个世界范围内的重大问题,而多数金属元素都表现不同程度的毒性,因此,适时准确分析生物和环境样品中痕量金属尤其是重金属元素的含量及其形态具有重要意义。
准确获取复杂基体样品系统中目标物(分子)的有效信息,是科学研究中的重要问题。然而在实际样品中基提效应会阻碍化学信息的获取,而且目标物浓度过低也会使化学信息的特征不明显。借助有效的分离富集技术,消除干扰基体,提高目标物浓度,是准确捕获有效信息的重要途径。而目前所能提供的样品分离富集理论与方法尚难以满足各类样品系统的需要。因此,建立样品预处理(分离富集)的新理论、新方法与检测技术,仍然是分析科学发展的瓶颈之一。
固相萃取是一种重要的样品预处理技术,其基本特点是试剂消耗少,富集倍数高,操作过程简单,所需费用低,更重要的是其容易实现自动化,从而得到了广泛关注和重视。不断地开发新型的萃取材料以及在原有材料的基础上进行适当的改性以期达到更好的萃取效果,是新型固相萃取技术的重要发展方向。
本论文以探索新型固相萃取方法为核心,以流动/顺序注射分析技术为进样手段,开发新型的固相萃取材料,研究新型的固相萃取方法或技术,建立固相萃取技术与原子光谱联用的新技术、新方法,并将其用于环境和生物样品中痕量金属元素/元素形态的分离分析。
论文第一章阐述了固相萃取技术的进展和现状以及固相萃取技术在痕量元素分离富集及形态分析中的应用。
论文第二章在顺序注射系统中采用竹炭微填充柱实现了痕量铋的分离富集,并将其与氢化物发生原子荧光光谱和电感耦合等离子体质谱联用,建立了在线固相萃取-氢化物发生原了荧光和等离子体质谱法测定痕量铋的方法。用标准物质CRM320(河床沉积物)验证了方法的准确性,并用两种检测方法分别对血液样品中的铋进行了测定,实验结果表明用原子荧光和等离子体质谱测定所得到的结果无明显差异。
论文第三章以木质纤维微填充柱为固相萃取及还原剂固定化的界面载体,以盐酸为反应试剂,实现了原位表面蒸气发生反应,建立了集分离富集,还原剂固定化和蒸气发生于一体的样品预处理系统,将该样品预处理系统与原子荧光光谱仪联用,建立了一种具有选择性较好,灵敏度和稳定性较高的痕量镉在线分离富集-蒸发生原子荧光检测方法。用标准水样SLRS-4和国家标准物质GBW08608验证了方法的准确性,对近海海水样品进行了测定,得到了满意的加标回收率。
论文第四章以涂覆在木质纤维表面的氢氧化镧沉淀为分离富集界面,基于共沉淀的原理实现了痕量硒(Ⅳ)的分离富集以及氢化物发生原子荧光光谱检测。以碱性洗脱剂洗脱回收富集的Se(Ⅳ),保证了氧氧化镧沉淀表面可反复使用。本方法有效地避免了常规共沉淀分离富集过程中共沉淀剂随待测组份一起洗脱所产生的基体效应,消除了后续检测中潜在的干扰因素。本方法可用于人发和大米(标准物质GBW10010)中痕量硒的检测以及水样中痕量硒的形态分析。
论文第五章以新合成的半胱氨酸功能化的纤维为富集材料,实现了痕量汞的分离富集及蒸气发生原子荧光检测。半胱氨酸的引入显著提高了纤维对痕量汞的吸附率,此相萃取方法与原子荧光联用有望实现痕量汞的形态分析。
The social and technological activities of human being have caused serious environmental pollution. Among the various pollutants, heavy metal species have attracted extensive attentions attributed to their toxicity. and this has been a worldwide problem. In this respect, it is highly necessary to provide timely warning of the accurate information about heavy metal accumulation in biological and environmental samples.
It is an important scientific issue to obtain useful information about the targets in complex sample matrixes. However, in real sample analysis, the presence of complex sample matrixes frequently blocks the determination of target species. In addition, in many cases the concentration of target is too low to be accurately quantified. Therefore, it is very often necessary to perform appropriate sample pretreatment by isolating the target from the sample matrixes, at the same time, preconcentration of the target species can be achieved. The present sample pretreatment theories and techniques are. however, not sufficient for various real sample matrixes. Thus, it is highly desrired to develop new theories and technologies of sample pretreatment, i.e., separation and preconcentration, in combination with suitable detection protocols.
Solid phase extraction is one of the most important sample pretreatment techniques which can provide high enrichment factors. It has some distinct featutes such as low sample and reagent consumption and thus low cost, ease of operation and automation. In this field, it is still highly desirable to develop novel adsorbent materials or modify the existing materials by introducing/immobilizing appropriate functional grupos in order to achieve better performances on the extraction of target species.
The present work aims at investigating novel solid phase extraction techniques based on flow injection/sequential injection, by developing new adsorbent material and sample pretreatment methodologies for trace metal species. In addition to use these methods for the analysis of heavy metals in biological and environmental sample matrixes by hyphenating the solid phase extraction protocols with detection by atomic spectrometry.
Chapter1discussed the state-of-the-art progresses of solid phase extraction techniques and their applications in the saparation/preconcentraion as well as speciation of heavy metal species in various samples.
In chapter2、the separation and preconcentration of bismuth was facilitated by employing a novel sequential injection system incorporating a mini-column packed with bamboo carbon followed by detection with hydride generation atomic fluorescence spectrometry and inductively coupled plasma mass spectrometry. The present system has been validated by analyzing a certified reference material of river sediment (CRM320), and spiking recovery of bismuth in human whole blood was performed by using hydride generation atomic fluorescence spectrometry. No significant difference was identified in the results of bismuth detection in blood samples by hyphenating the present solid extraction extraction system with detection by hydride generation atomic fluorescence spectrometry and inductively coupled plasma mass spectrometry.
Chapter3of the thesis developed a sequential injection sample pretreatment procedure with a cellulose fibre packed micro-column as adsorbent for the separation and preconcentration of ultra-trace cadmium with detection by atomic fluorescence spectrometry. The cellulose fibre surface was used to integrate the preconcentration of cadmium, the immobilization of reducing reagent (NaBH4), the elution of cadmium and the ensuing on-surface vapor generation by reaction with hydrochloric acid. The present investigation provides a sensitive, selective and stable system for on-line separation/preconcentration of cadmium. The procedure was validated by analyzing certified reference materials of Riverine Water SLRS-4and Trace Elements in Water (GBW08608), in addition to spiking recovery in a coastal sea water.
In chapter4, lanthanum hydroxide precipitate is for the first time coated onto cellulose fibre and serves as a novel sorption medium for separation and speciation of inorganic selenium. The retained selenium(Ⅳ) was eluted from the micro-column packed with precipitate layer coated cellulose fibre and determined by atomic fluorescence spevtrometry. The elution of the retained selenium by using an alkaline medium avoids the dissolution of the precipitate for each analysis run in a routine precipitation/co-precipitation-based separation and preconcentration system, and thus, eliminates potential interfering effects for the detection or post-derivatization process arisen from the bulk of the precipitate and ensures repetitive use of the coated precipitate layer and improves its lifetime. The procedure is validated by analyzing selenium in a reference material GBW10010(rice) and a human hair sample. The procedure is further demonstrated by speciation of inorganic selenium in surface water samples by pre-reduction of selenate.
In the last chapter, a novel cellulose fibre functionalized with cysteine was prepared as adsorbent for the collection of mercury, and a procedure for separation and preconcentraton of mercury was developed by coupling with vapor generation atomic fluorescence spectrometry. The thiol group in cysteine molecule immobilized on the cellulose fibre significantly improved the sorption capability for mercury attributed to the affinity of thiol for mercury. It is potentially feasible for the speciation of inorganic and organic mercury by coupling solid phase extraction using the present cysteine funationalized cellulose fibre with detection by atomic fluorescence spectrometry.
准确获取复杂基体样品系统中目标物(分子)的有效信息,是科学研究中的重要问题。然而在实际样品中基提效应会阻碍化学信息的获取,而且目标物浓度过低也会使化学信息的特征不明显。借助有效的分离富集技术,消除干扰基体,提高目标物浓度,是准确捕获有效信息的重要途径。而目前所能提供的样品分离富集理论与方法尚难以满足各类样品系统的需要。因此,建立样品预处理(分离富集)的新理论、新方法与检测技术,仍然是分析科学发展的瓶颈之一。
固相萃取是一种重要的样品预处理技术,其基本特点是试剂消耗少,富集倍数高,操作过程简单,所需费用低,更重要的是其容易实现自动化,从而得到了广泛关注和重视。不断地开发新型的萃取材料以及在原有材料的基础上进行适当的改性以期达到更好的萃取效果,是新型固相萃取技术的重要发展方向。
本论文以探索新型固相萃取方法为核心,以流动/顺序注射分析技术为进样手段,开发新型的固相萃取材料,研究新型的固相萃取方法或技术,建立固相萃取技术与原子光谱联用的新技术、新方法,并将其用于环境和生物样品中痕量金属元素/元素形态的分离分析。
论文第一章阐述了固相萃取技术的进展和现状以及固相萃取技术在痕量元素分离富集及形态分析中的应用。
论文第二章在顺序注射系统中采用竹炭微填充柱实现了痕量铋的分离富集,并将其与氢化物发生原子荧光光谱和电感耦合等离子体质谱联用,建立了在线固相萃取-氢化物发生原了荧光和等离子体质谱法测定痕量铋的方法。用标准物质CRM320(河床沉积物)验证了方法的准确性,并用两种检测方法分别对血液样品中的铋进行了测定,实验结果表明用原子荧光和等离子体质谱测定所得到的结果无明显差异。
论文第三章以木质纤维微填充柱为固相萃取及还原剂固定化的界面载体,以盐酸为反应试剂,实现了原位表面蒸气发生反应,建立了集分离富集,还原剂固定化和蒸气发生于一体的样品预处理系统,将该样品预处理系统与原子荧光光谱仪联用,建立了一种具有选择性较好,灵敏度和稳定性较高的痕量镉在线分离富集-蒸发生原子荧光检测方法。用标准水样SLRS-4和国家标准物质GBW08608验证了方法的准确性,对近海海水样品进行了测定,得到了满意的加标回收率。
论文第四章以涂覆在木质纤维表面的氢氧化镧沉淀为分离富集界面,基于共沉淀的原理实现了痕量硒(Ⅳ)的分离富集以及氢化物发生原子荧光光谱检测。以碱性洗脱剂洗脱回收富集的Se(Ⅳ),保证了氧氧化镧沉淀表面可反复使用。本方法有效地避免了常规共沉淀分离富集过程中共沉淀剂随待测组份一起洗脱所产生的基体效应,消除了后续检测中潜在的干扰因素。本方法可用于人发和大米(标准物质GBW10010)中痕量硒的检测以及水样中痕量硒的形态分析。
论文第五章以新合成的半胱氨酸功能化的纤维为富集材料,实现了痕量汞的分离富集及蒸气发生原子荧光检测。半胱氨酸的引入显著提高了纤维对痕量汞的吸附率,此相萃取方法与原子荧光联用有望实现痕量汞的形态分析。
The social and technological activities of human being have caused serious environmental pollution. Among the various pollutants, heavy metal species have attracted extensive attentions attributed to their toxicity. and this has been a worldwide problem. In this respect, it is highly necessary to provide timely warning of the accurate information about heavy metal accumulation in biological and environmental samples.
It is an important scientific issue to obtain useful information about the targets in complex sample matrixes. However, in real sample analysis, the presence of complex sample matrixes frequently blocks the determination of target species. In addition, in many cases the concentration of target is too low to be accurately quantified. Therefore, it is very often necessary to perform appropriate sample pretreatment by isolating the target from the sample matrixes, at the same time, preconcentration of the target species can be achieved. The present sample pretreatment theories and techniques are. however, not sufficient for various real sample matrixes. Thus, it is highly desrired to develop new theories and technologies of sample pretreatment, i.e., separation and preconcentration, in combination with suitable detection protocols.
Solid phase extraction is one of the most important sample pretreatment techniques which can provide high enrichment factors. It has some distinct featutes such as low sample and reagent consumption and thus low cost, ease of operation and automation. In this field, it is still highly desirable to develop novel adsorbent materials or modify the existing materials by introducing/immobilizing appropriate functional grupos in order to achieve better performances on the extraction of target species.
The present work aims at investigating novel solid phase extraction techniques based on flow injection/sequential injection, by developing new adsorbent material and sample pretreatment methodologies for trace metal species. In addition to use these methods for the analysis of heavy metals in biological and environmental sample matrixes by hyphenating the solid phase extraction protocols with detection by atomic spectrometry.
Chapter1discussed the state-of-the-art progresses of solid phase extraction techniques and their applications in the saparation/preconcentraion as well as speciation of heavy metal species in various samples.
In chapter2、the separation and preconcentration of bismuth was facilitated by employing a novel sequential injection system incorporating a mini-column packed with bamboo carbon followed by detection with hydride generation atomic fluorescence spectrometry and inductively coupled plasma mass spectrometry. The present system has been validated by analyzing a certified reference material of river sediment (CRM320), and spiking recovery of bismuth in human whole blood was performed by using hydride generation atomic fluorescence spectrometry. No significant difference was identified in the results of bismuth detection in blood samples by hyphenating the present solid extraction extraction system with detection by hydride generation atomic fluorescence spectrometry and inductively coupled plasma mass spectrometry.
Chapter3of the thesis developed a sequential injection sample pretreatment procedure with a cellulose fibre packed micro-column as adsorbent for the separation and preconcentration of ultra-trace cadmium with detection by atomic fluorescence spectrometry. The cellulose fibre surface was used to integrate the preconcentration of cadmium, the immobilization of reducing reagent (NaBH4), the elution of cadmium and the ensuing on-surface vapor generation by reaction with hydrochloric acid. The present investigation provides a sensitive, selective and stable system for on-line separation/preconcentration of cadmium. The procedure was validated by analyzing certified reference materials of Riverine Water SLRS-4and Trace Elements in Water (GBW08608), in addition to spiking recovery in a coastal sea water.
In chapter4, lanthanum hydroxide precipitate is for the first time coated onto cellulose fibre and serves as a novel sorption medium for separation and speciation of inorganic selenium. The retained selenium(Ⅳ) was eluted from the micro-column packed with precipitate layer coated cellulose fibre and determined by atomic fluorescence spevtrometry. The elution of the retained selenium by using an alkaline medium avoids the dissolution of the precipitate for each analysis run in a routine precipitation/co-precipitation-based separation and preconcentration system, and thus, eliminates potential interfering effects for the detection or post-derivatization process arisen from the bulk of the precipitate and ensures repetitive use of the coated precipitate layer and improves its lifetime. The procedure is validated by analyzing selenium in a reference material GBW10010(rice) and a human hair sample. The procedure is further demonstrated by speciation of inorganic selenium in surface water samples by pre-reduction of selenate.
In the last chapter, a novel cellulose fibre functionalized with cysteine was prepared as adsorbent for the collection of mercury, and a procedure for separation and preconcentraton of mercury was developed by coupling with vapor generation atomic fluorescence spectrometry. The thiol group in cysteine molecule immobilized on the cellulose fibre significantly improved the sorption capability for mercury attributed to the affinity of thiol for mercury. It is potentially feasible for the speciation of inorganic and organic mercury by coupling solid phase extraction using the present cysteine funationalized cellulose fibre with detection by atomic fluorescence spectrometry.
引文
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