固相微萃取技术与环境样品前处理

固相微萃取技术是80 年代末发展起来的一项新型的无溶剂化环境样品前处理技术, 它主要与气相色谱和高效液相色谱联用, 能快速和有效地分析环境样品中的痕量有机污染物。技术从出现至今主要在萃取装置(萃取纤维涂层)、萃取方式及后序分析仪器上有较大的发展和变化, 这使得技术的应用范围不断拓宽。通过对现有文献的总结, 本文还提出了固相微萃取技术今后的发展趋势。     

新型的样品前处理技术-固相微萃取

文中对固相微萃取,作为一种试样预处理的新技术,在1990-2004年的进展作了评述,介绍了固相微萃取技术的装置、试验方法、原理、涂层、影响因素、应用及发展趋势,引用文献39篇。     

固相萃取-气相色谱-质谱法测定纺织品中全氟辛烷磺酸盐

采用固相萃取-气相色谱-质谱法测定纺织品中全氟辛烷磺酸盐的含量。纺织品样品在索氏提取器中用甲醇提取后,经固相萃取净化,并用盐酸溶液酸化,再与四丁基氢氧化铵反应。在气相色谱分离中用HP-5MS毛细管柱为固定相,在质谱分析中采用全扫描和选择离子监测模式。全氟辛烷磺酸盐的质量浓度在1.0~30.0mg·kg-1范围内与其峰面积呈线性关系,方法的检出限(3S/N)为0.13mg·kg-1。加标回收率在88.8%~91.1%之间,测定值的相对标准偏差在均小于5.0%。     

应用于全氟辛烷磺酸萃取富集的全氟癸基修饰毛细管硅胶整体柱的制备及应用

利用溶胶-凝胶法,经过烷氧基硅烷的水解、硅羟基的缩聚、凝胶化、陈化、中孔制备、干燥和表面修饰等步骤制备了全氟癸基修饰的毛细管硅胶整体柱。采用该整体柱对全氟辛烷磺酸(PFOS)进行萃取富集,考察其富集特性和效率,并与传统的C18毛细管硅胶整体柱进行对比。结果表明,全氟癸基修饰毛细管硅胶整体柱(15 cm×75 μm)对PFOS具有更高的吸附量和更好的富集选择性,其平均吸附量可以达到75 ng;样品中PFOS的质量浓度为0.25 mg/L时,富集倍数平均可以达到29倍。此全氟癸基修饰毛细管硅胶整体柱对PFOS具有良好的萃取富集性能,可用于水质中痕量PFOS的萃取富集。     

应用于全氟辛烷磺酸萃取富集的全氟癸基修饰毛细管硅胶整体柱的制备及应用

利用溶胶-凝胶法,经过烷氧基硅烷的水解、硅羟基的缩聚、凝胶化、陈化、中孔制备、干燥和表面修饰等步骤制备了全氟癸基修饰的毛细管硅胶整体柱。采用该整体柱对全氟辛烷磺酸(PFOS)进行萃取富集,考察其富集特性和效率,并与传统的C18毛细管硅胶整体柱进行对比。结果表明,全氟癸基修饰毛细管硅胶整体柱(15 cm×75μm)对PFOS具有更高的吸附量和更好的富集选择性,其平均吸附量可以达到75 ng;样品中PFOS的质量浓度为0.25 mg/L时,富集倍数平均可以达到29倍。此全氟癸基修饰毛细管硅胶整体柱对PFOS具有良好的萃取富集性能,可用于水质中痕量PFOS的萃取富集。     

新一代萃取分离技术──固相微萃取

介绍了一种新型样品制备法——固相做萃取（SPME）的原理及其应用。与其它样品制备技术相比,SPME法具有操作时间短、样品量小、无需萃取溶剂、适于分析挥发性与非挥发性物质、重视性好等优点。     

薄膜固相微萃取技术的应用进展

随着样品前处理方法的快速发展,薄膜固相微萃取（TFME）技术已经逐渐成为样品前处理领域的基础性研究课题,同时相关的联用方法也受到广泛关注。与其他样品前处理方法相比,TFME具有较高的表面积体积比,以及较大的有效萃取体积,因此可在提高灵敏度的同时减少萃取时间。TFME法结合其他样品分析方法可广泛用于违禁药物、爆炸物、有机农药、兽药等物质的分析中,同时在药物、食品、环境分析等领域有广泛的应用。该文概述了TFME技术的萃取原理及多样化的萃取器件,综述了TFME技术与多项不同分析仪器的联用技术,并展望其发展趋势。     

固相微萃取研究进展

对固相微萃取的发展背景，应用及其研究进展作了综述。引用文献 145篇。     

典型全氟有机酸类化合物的样品前处理与分析方法研究进展

全氟辛烷磺酸（PFOS）和全氟辛烷羧酸（PFOA）是两种典型的全氟有机酸类化合物,也是全氟化合物（PFCs）前体物的最终降解产物,具有肝毒性、胚胎毒性、生殖毒性、神经毒性,检出率最高。在各种被污染的介质中,PFOS和PFOA含量往往很低,基体复杂多样,快速高效的样品前处理技术成为测定的关键环节。目前,国际上对PFOS和PFOA的测定无统一标准,而我国关于PFCs的分析研究落后于国际发展水平。该文介绍了PFOS和PFOA的特性,系统总结和评述了前处理技术（液液萃取、固相萃取、固相微萃取、超声萃取和QuEChERS法）及分析方法（色谱-质谱方法、光谱法、酶联免疫法和电化学法）,以期为PFOS和PFOA的分析监测及标准制定提供参考。     

固相微萃取-液相色谱联用技术研究进展

本文较系统地介绍了固相微萃取-液相色谱联用技术的原理、特点、发展现状及其发展趋势,并对该技术在样品前处理尤其是环境样品前处理中的应用作了较详细的综述     

固相微萃取在药品和生物样品分析中的应用

 按被分析的样品的性质分类 ,对 2 0世纪 90年代发展起来的一种新型样品预处理技术固相微萃取技术在药品及生物样品分析中的应用实例进行了综述 ,共 6 0篇。     

用于化学毒剂检测的微萃取技术研究进展

对化学毒剂及其降解产物的分析检测是准确鉴别化学沾染的重要手段.由于化学毒剂及其降解产物的样品可能存在于各种基质中,且部分化学毒剂在水体等基质中降解速度过快,所以将痕量样品从复杂基质中快速高效的富集提取出来显得尤其重要.微萃取技术具有装置体积小、使用少量或不使用溶剂、绿色环保、易与色谱分析技术联用等突出优势受到广泛的关注...     

Gold nanoparticles based solid‐phase microextraction coatings for determining organochlorine pesticides in aqueous environmental samples

The use of solid‐phase microextraction coatings based on gold nanoparticles was investigated, focusing the attention on the preparation of nanoparticles with nonclassical reduction agents of HAuCl₄ such as gallic acid and H₂O₂, rather than the conventional sodium citrate. All nanoparticles were characterized by diode array spectroscopy, whereas novel nanoparticles prepared with gallic acid and H₂O₂ were also characterized by microscopic techniques. Solid‐phase microextraction coatings were prepared with a layer‐by‐layer approach. Gallic acid permitted the preparation of stable nanoparticles with milder experimental conditions (1 min, room temperature) and provided the most uniform coatings (thickness ∼3 μm). Seven organochlorine pesticides were determined in different environmental waters using gas chromatography with electron capture detection. Despite the low thickness of the coatings, limits of detection of the entire method down to 0.13 μg/L were obtained. A comparison with the commercial polyacrylate in terms of the partition coefficients of the analytes to the coatings gave logarithm of the partition coefficient values two times higher with gallic acid than polyacrylate (although the commercial fiber is 28 times thicker). Interfiber relative standard deviation values ranged from 8.67 to 21.3%. Optimum fibers also presented an adequate lifetime (>100 extractions).     

Solid‐phase microextraction for the human biomonitoring of environmental chemicals: Current applications and future perspectives

Sample preparation is one of the crucial steps in the analytical chemistry including human biomonitoring studies. Although there are several traditional approaches available, solid‐phase microextraction is emerged as one of the pioneering techniques due to its simplicity, rapidness, wide applicability, and miniaturization of traditional sample preparation (e.g., use of less or no organic solvents). There are few earlier review articles available on the advancements in solid‐phase microextraction and its use for the measurement of environmental chemicals in various types of environmental samples. However, a collective information on applicability and current usage of solid‐phase microextraction for the human biomonitoring of environmental chemicals are scarce, nonetheless, rising demands on innovative analytical approaches for human biomonitoring studies. Hence, in this review article, we covered the application of solid‐phase microextraction as extraction/purification methods for more than 15 classes of environmental chemicals to assess their respective exposure levels and associated health outcomes in various human population reported across the globe. Further, a detailed discussion on various types of matrix used, nature of coupled analytical instrumentations, and limitations and future perspectives of solid‐phase microextraction for human biomonitoring studies is presented in this review.     

固相微萃取新技术

 固相微萃取是基于萃取涂层与样品之间的吸附 /溶解 解吸平衡而建立起来的集进样、萃取、浓缩功能于一体的技术。综述了固相微萃取技术的最新发展动态 ,介绍了管内 (in tube)固相微萃取、新型萃取头以及固相微萃取与其他分析技术的联用情况。     

采用溶胶-凝胶技术涂层的新型固相微萃取方法及其应用

将溶胶-凝胶技术应用于SPME固相涂层的制备,涂制的端羟基-聚二甲基硅氧烷固相涂层热稳定性好,萃取时间和解吸时间短,对极性化合物及非极性化合物均有较强的萃取富集能力。扫描电镜图显示涂层表面为多孔结构。采用该涂层的SPME方法在对环境样品的分析中获得了令人满意的效果。     

Analysis of trace‐level nitrated polycyclic aromatic hydrocarbons in water samples by solid‐phase microextraction with gas chromatography and mass spectrometry

A solid‐phase microextraction coupled with gas chromatography and mass spectrometry method has been developed for the determination of ten nitrated polycyclic aromatic hydrocarbons in water samples. Five different kinds of commerical fibers were used to compare the extraction efficiency, including 65 μm polydimethylsiloxane/divinylbenzene, 100 μm polydimethylsiloxane, 30 μm polydimethylsiloxane, 7 μm polydimethylsiloxane, and 85 μm polyacrylate fibers. Five factors were also selected to optimize conditions, including extraction temperature, time, stirring speed, salt concentration, and headspace volume. Taguchi design was applied to design the experiments and obtain the best parameters. The results show that 65 μm polydimethylsiloxane/divinylbenzene fiber directly immersed into aqueous solution for 35 min at 55°C with a constant stirring rate of 1150 rpm were the optimal conditions. Under these conditions, the limits of quantification were 0.007–0.063 μg/L, and the relative standard deviation based on six replicates ranged from 2.8 to 9.5%. The spiked recoveries ranged from 69.1 to 110.1%. Intra‐ and inter day relative standard deviations at three concentration levels were less than 12%, and the recoveries were 66.4–111.5%. The proposed method is reliable for analyzing nitrated polycyclic aromatic hydrocarbons in different water samples.     

Analysis of mono-nitrotoluenes in water samples by using nano-structured polypyrrol as a sorbent of solid-phase microextraction

Nano-structured polypyrrole (PPY) was used as a coating of solid-phase microextraction (SPME) fibre to increase the extraction efficiency of headspace solid phase microextraction (HS-SPME) of mono-nitrotoluene (MNT) isomers in water samples. The nano-structured PPY was prepared electrochemically by template-free method in the presence of dodecylbenzene sulphonate (DBS) as dopant. Nano-fibrous structures of PPY with a diameter in the range of 38–129 nm were obtained. The porous surface structure of the film, revealed by scanning electron microscopy (SEM), provided high surface areas and allowed for high extraction efficiency of MNT isomers. The extraction procedure was optimised by selecting the appropriate extraction parameters including the time and temperature of adsorption, salt concentration and stirring rate. The calibration graphs obtained by HS-SPME using the proposed fibre followed by GC-FID analysis were linear in a concentration range of 0.1–500 µg L^?1 (r > 0.999) with detection limits below 0.012 µg L^?1 for three isomers. Repeatability of the method was less than 6% (RSD%, n = 4). Good recoveries (88–108%) were obtained for the extraction of mono-nitrotoluenes in real water samples.