环境样品前处理技术及其进展（二）

在前文中讨论了环境样品的制备、前处理的概况，以及超临界流体萃取法。本文将继续报导近年来环境样品制备与前处理领域中其他一些新技术和新方法，包括固相萃取（ＳＰＥ）、微波溶出（ＭＷＤ）和液膜萃取（ＳＬＭ）法，阐述了这些方法的基本原理、操作过程、各种实验参数的影响，及其在环境样品制备与前处理中的应用，并探讨了该领域的发展动向。     

应用活性炭纤维型固相微萃取器定量分析化妆品中的甲醇

固相微萃取技术（Solid—Phase Micro—Extraction,SPME）是二十世纪八十年代末发展起来的一项新型无溶剂化样品前处理技术,该方法解决了传统环境样品前处理技术中使用大量有机溶剂、处理时间长、操作步骤多等缺点,成为当今环境分析化学的研究热点之一．     

环境样品中汞形态分析技术的进展

汞的毒性、环境行为、生物有效性不仅跟其浓度有关,还决定于其化学形态,因此汞的形态分析在环境科学中具有重要意义。样品前处理几乎是汞形态分析研究中不可或缺的步骤,而色谱和光谱/质谱联用技术是目前普遍采用的分离检测方法。文章对近十年来这些方面的研究进展进行了综述,主要包括样品的前处理方法如酸/碱溶剂萃取、微波辅助萃取、固相萃取、固相微萃取、单滴微萃取、分散液液微萃取等,以及色谱（液相色谱、气相色谱）和毛细管电泳与光谱/质谱（紫外可见光谱、原子吸收光谱、原子荧光光谱、等离子体质谱等）的联用技术在汞化合物形态分析中的应用情况。最后提出今后应重点研究建立高效、简便的前处理方法,发展高分离度、高灵敏度、高速度的分离检测联用技术,以便更好地对汞的形态进行分析监测。     

超临界流体萃取在研究土壤和沉积物结合态残留中的应用

许多有机污染物在土壤和沉积物中形成持久稳定的结合态残留；结合态残留对土壤和沉积物的解毒过程、污染物长期分配行为、生物可用性和生物毒性都具有重要影响。为了揭示结合态残留的形成机制及其对污染物环境行为和毒理学参数的影响，从土壤或沉积物中提取出不同结合状态的有机污染物就显得非常重要。超临界流体萃取(SFE)可以实现选择性萃取，从而得到有关污染物一基体间相互作用的信息。文章介绍了SFE应用类型、超临界流体种类以及影响SFE萃取率的因素，对SFE模拟有机污染物长期吸附／解吸行为和生物可用性研究进行了论述，并认为SFE势必发展成为土壤或沉积物中结合态残留形成机理研究、土壤修复和生态风险评价的一种强有力的技术。     

加速溶剂萃取的原理及应用

复杂样品的前处理,常常是现代分析方法的薄弱五一节,在以往的数年中,人们做了多种尝试以期找到一种高效、快捷的方法以取代传统的萃取法,例如,自动索氏萃取、微波消解、超声萃取和超临界萃取等。值得注意的是,以上各法无论是自动索氏萃取,还是超临界流体萃取……等,都有一个共同点,即与温度有关,在萃取过程中,通过适当提高温度,可以获得较好的结果,例如,在自动索氏萃取中,由于萃取时是将样品浸入沸腾的溶剂之中,因此,其萃取速度和效率较常规索氏萃取法快且溶剂用量少,超临界流体萃取可通过提高萃取时的温度使其温度使其回收率得到改善,而微波萃取则是利用一种可以施加压力的容器,将溶剂加热到其沸点之上,来提高其萃取的效率,虽然以上各法与经典的索种可以施加压力的容器,将溶剂加热到其沸点之上,来提高其萃取的效率,虽然以上各法与经典的索氏法相比已有了很大的进步,但有机溶剂的用量仍然偏多,萃取时间较长,萃取效率还不够高。     

同位素稀释-液相色谱串联质谱法测定固相萃取柱中5种双酚A、壬基酚和辛基酚类化合物

双酚A（Bisphenol A）、壬基酚（Nonylphenol）和辛基酚（Octylphenol）是环境中常见的几种内分泌干扰物质,对生态环境和人类健康造成一定的危害.由于这类物质在实际样品中含量通常较低（ng.L-1级）,样品基体对测定可能会有一定的干扰,因此准确测定时往往需要对样品进行萃取、净化和浓缩等前处理.固相萃取因具有易于操作、适用性广、     

多环芳烃的样品前处理技术研究进展

多环芳烃(PAHs)是一类致癌、致畸、致突变的持久性有机物污染物,广泛存在于大气、水、土壤和生物等介质中.由于PAHs基体复杂并且含量很低,所以样品的净化和富集尤为重要.本文综述了近5年来国内外有关PAHs的样品前处理技术和方法的基本原理和代表性应用,包括液相微萃取、分散液液微萃取、固相微萃取、搅拌子吸附萃取、微耗损固相微萃取、分散固相微萃取法,比较了各方法的优缺点,并对PAHs的样品前处理技术的发展进行了展望.     

环境样品中汞形态分析技术的进展

汞的毒性、环境行为、生物有效性不仅跟其浓度有关,还决定于其化学形态,因此汞的形态分析在环境科学中具有重要意义。样品前处理几乎是汞形态分析研究中不可或缺的步骤,而色谱和光谱/质谱联用技术是目前普遍采用的分离检测方法。文章对近十年来这些方面的研究进展进行了综述,主要包括样品的前处理方法如酸/碱溶剂萃取、微波辅助萃取、固相萃取、固相微萃取、单滴微萃取、分散液液微萃取等,以及色谱(液相色谱、气相色谱)和毛细管电泳与光谱/质谱(紫外可见光谱、原子吸收光谱、原子荧光光谱、等离子体质谱等)的联用技术在汞化合物形态分析中的应用情况。最后提出今后应重点研究建立高效、简便的前处理方法,发展高分离度、高灵敏度、高速度的分离检测联用技术,以便更好地对汞的形态进行分析监测。     

加速溶剂萃取技术及其在环境分析中的应用

加速溶剂萃取技术是一项新颖的样品前处理技术，通过升高温度与压力结合使用有机溶剂，可快速，有效地由基体中萃取各种欲测物。本文系统地阐述了该技术的基本原理，各种影响因子及其在环境分析中的应用。该法适用于固体和半固体样品的前处理。     

浊点萃取技术在环境样品痕量元素分析中的应用研究进展

浊点萃取法是近年来发展起来的一种绿色环保的样品前处理技术.本文详细介绍了浊点萃取方法的原理,对国内外近5年来(2008年—至今)利用浊点萃取与几种常见的原子光谱分析仪器以及与电感耦合等离子体质谱仪联用技术,在环境样品中痕量元素分离和富集以及形态分析中的应用研究进展进行了评述.同时对浊点萃取技术目前的最新发展方向、尚存在的问题以及发展前景进行了逐一探讨.     

典型有机磷酸酯阻燃剂分析方法研究进展

有机磷酸酯(OPEs)是一类重要的有机磷阻燃剂,近些年逐渐取代了溴代阻燃剂,广泛应用于各行各业,也因此导致在多种环境介质中有较高的暴露量和潜在风险。已有研究表明,OPEs具有一定的毒理效应,对人体及其他生物均有潜在危害。本文综述了近年来国内外OPEs的检测技术,详述了不同环境介质OPEs的前处理方法。结果表明,目前固相萃取(SPE)和固相微萃取(SPME)仍是水样前处理的主要方法;对于固体样品,加速溶剂萃取/加压液相萃取(ASE/PLE)和微波辅助萃取(MAE)应用较多;虽然大气样品仍以固体吸附剂方式为主,但已向在线一体化方向发展;而生物样品的前处理方法多与水样和固体样品方法相似;但是对于复杂环境介质中OPEs样品的前处理较为困难,方法有待改善;气相色谱-质谱联用(GC-MS)和气相色谱-氮磷检测器(GC-NPD)对弱极性和易挥发的OPEs分析效果好,而强极性和难挥发的OPEs多用液相色谱-质谱联用(LCMS);气相色谱-质谱串联(GC-MS/MS)、液相色谱-质谱串联(LC-MS/MS)和高效液相色谱-质谱串联(UPLC-MS/MS)等对多种复杂的环境介质中的OPEs均有较好的检测分析效果,但并未普及。最后,对OPEs分析测试方法的发展趋势提出了展望。     

Biosorbents for solid-phase extraction of toxic elements in waters

Some trace metals are highly toxic for the environment. There is therefore a need for reliable methods for the determination of metals at trace levels. To this end, new sample pretreatment methods such as separation, preconcentration and speciation prior to the determination of metal ions have developed rapidly. Biosorption has become a major tool for solid-phase extraction methods. This review covers selected biosorbents such as algae, bacteria, filamentous fungi and yeasts, as new sorbents used in the solid-phase extraction of metal ions from various water sample matrices. A survey of the literature over 2004-2014 shows possible applications of selected new sorbents available for use in trace metal analysis in waters using solidphase extraction. We highlight the preconcentration of the toxic elements prior to their determination by atomic spectrometry.     

Modified pretreatment method for total microbial DNA extraction from contaminated river sediment

Extraction of high-quality microbial DNA from contaminated environmental samples is an essential step in microbial ecological study. Based on previously published methods for soil and sediment samples, a modified pretreatment method was developed for extracting microbial DNA from heavily contaminated river sediment samples via selection of optimal pretreatment parameters (i.e., reagent solution, reaction duration, and temperature). The pretreatment procedure involves washing the river sediment sample for three times with a solution containing 0.1 mol·L^-1 ethylene diamine tetraacetic acid (EDTA), 0.1 mol·L^-1 Tris (pH 8.0), 1.5 mol·L^-1 NaCl, 0.1 mol·L^-1 NaH₂PO₄, and Na₂HPO₄ at 65°C with 180 r·min^-1 for 15 min to remove humic materials and heavy metals prior to the employment of standard DNA extraction procedures. We compared the results of standard procedure DNA extraction following pretreatment, without pretreatment, and with using a commercial PowerSoil^TM DNA Isolation Kit. The results indicated that the pretreatment significantly improved the DNA quality based on DNA yield, DNA fragment length, and determination of prokaryotic diversity. Prokaryotic diversity exhibited in the DNA with the pretreatment was also considerably higher than that extracted with the PowerSoil^TM DNA Isolation Kit only. The pretreatment method worked well even with a small amount of sediment sample (0.25 g or even lower). The method provides a novel, simple, cost-effective tool for DNA extraction for microbial community analysis in environmental monitoring and remediation processes.     

大气有机污染物的吸附剂富集—超临界流体萃取—色质联用分析

本文研究了有机吸附剂ＧＤＸ－１０１１，ＧＤＸ－１０２，ＧＤＸ－５０２富集大气中痕量有机污染物的超临界流全萃取方法，比较了三种吸附剂富集大气中有机物的主要成分其超临界流体的萃取效率，并与索钉抽提法做了对比，结果表明，ＧＤＸ－５０２吸附有机物组分最多，超临界流体萃取对ＧＤＸ－５０２的解吸效率也最高，对被ＧＤＸ－５０２吸附的可以定量分析的３５种有机物的平均回收率为８４．５－１０８．９％，相对标准偏差为１     

Conversion of waste plastics into value-added carbon materials

Plastic pollution is a major environmental issue worldwide, calling for advanced methods to recycle waste plastics in the context of the circular economy. Here we review methods and strategies to convert waste plastics into value-added carbon materials, with focus on sources, properties, pretreatment of waste plastics, and on preparation of carbon materials. Pretreatment techniques include mechanical crushing, plastic stabilization and electrospinning. Carbon materials such as carbon nanotubes, graphene, carbon nanosheets, carbon spheres and porous carbon are prepared by oxygen-limited carbonization, catalytic carbonization, the template-based method, and pressure carbonization. We emphasize the conversion of polyethene terephthalate, polyethylene, polypropylene, polystyrene, halogenated plastics, polyurethane and mixed plastics.

     

An evaluation of procedures for the digestion of soils and vegetation from areas with metalliferous pollution

Various digestion or extraction processes are available for the determination of trace metals in environmental samples using diverse analytical techniques. Our research examines the most efficient and reproducible methods of digestion utilising readily available laboratory equipment, reagents and instrumentation. Extraction procedures reported in over 80 recent research works were considered and the most common methods were critically evaluated. Thus nitric acid, nitric acid/perchloric acid, aqua regia, nitric acid/hydrogen peroxide and microwave-assisted methods were investigated using soil and leaf samples collected adjacent to three old metalliferous workings. Analysis was carried out using Flame Atomic Absorption Spectrometry and the results were evaluated. Differences in efficiency of extraction relative to specific metals and different substrates are highlighted and recommendations made for a digestion procedure suitable for environmental samples. Aqua regia produced the most accurate, efficient and reproducible results; we consider methods of improving both of these factors and sample preparation. Our recommended methodology has applications in environmental surveys, environmental geology, environmental toxicology, geochemistry and provides a means of obtaining meaningful and reliable results for the determination of metals present in soils, minerals and vegetation.     

Voltammetric analysis of metallothioneins and copper (II) in fish for water biomonitoring studies

An major research area in environmental chemistry is the development of methods for the analysis of biomarkers. Metallothioneins are used as biomarkers in studies of heavy metals exposure in water, because metallothioneins are synthesized and accumulated when organisms are exposed to toxic concentrations of pollutants. In this work, simple and sensitive voltammetric methods were developed for metallothionein and copper (II) determinations in fish liver Lepomis gibbosus. Both analytical methodologies were optimized and applied to samples extracted from individuals previously submitted to sub-lethal toxicological trials with copper sulphate (CuSO₄) and cadmium chloride (CdCl₂). The obtained results showed that both methods are very precise, sensitive, and involve simple sample preparation processes. Moreover, metallothioneins showed better correlation with the toxic exposure than Cu²⁺. To the best of our knowledge, this is the first time that hepatic metallothioneins and Cu²⁺ contents are voltammetrically determined in order to be compared in their function as heavy metal biological indicators.