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采用溶胶-凝胶技术涂层的新型固相微萃取方法及其应用 总被引:13,自引:0,他引:13
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。 相似文献
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本文对葫芦脲(CB)作为一种新型固相微萃取(SPME)涂层材料进行了研究并用于中药白豆蔻的气相色谱分析测定.本文采用的CB SPME涂层制备方法简便、快速,并具有良好的热稳定性和重复性.CB[6]SPME萃取得到的主要成分与水蒸气蒸馏(SD)法基本一致,并且CB[6]SPME对色谱后流出的目标成分的相对峰面积比明显高于SD法和商品SPME萃取材料PDMS/CAR和PDMS/DVB,这可能是由于葫芦脲的特殊分子结构及其与组分分子间选择性作用所致.葫芦脲作为一种新型SPME涂层材料具有很大的研究潜力和应用前景. 相似文献
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用于固相微萃取的乙烯基开链冠醚复合涂层的研制 总被引:2,自引:0,他引:2
固相微萃取 (SPME)是一种新型的样品预处理技术 [1] ,其核心是 SPME装置中萃取头上的固相涂层 .目前商用 SPME涂层的种类较少 ,热稳定性较差 (推荐使用温度 2 0 0~ 2 80℃ ) ,使用寿命较短(40~ 1 0 0次 ) ,价格偏高 ,限制了其推广应用 .因此发展高选择性、高稳定性和高效的固 相似文献
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固相微萃取(Solid-phase microextraction,SPME)技术因其具有操作简单、萃取时间短、无需有机溶剂、易于自动化操作等优点,成为近年来发展起来的一种新型样品前处理技术。涂层是SPME技术的核心,决定了涂层萃取的选择性和容量。离子液体和聚离子液体因具有环境友好、蒸汽压低、热稳定性好、设计灵活、粘度大等特点,已作为一类新的涂层材料广泛应用于SPME,并对各种分析物均展现出良好的萃取效果和选择性。本文从制备技术、形貌、选择性、稳定性、寿命、应用等方面综述了近年来离子液体和聚离子液体基SPME涂层的研究进展,对它们的优缺点进行了对比讨论,并对其未来发展方向进行了展望。 相似文献
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样品的提取是法庭科学分析中至关重要的一步,尤其是在处理各种复杂基质(如土壤、生物样品、火灾残留物等)中痕量和超痕量的目标分析物时。传统样品前处理技术如索氏提取、液液萃取等,步骤繁琐,耗时耗力,过程中易造成样品的损失和二次污染,且萃取所需的大量溶剂还会对环境及研究人员的健康构成威胁。为此,无需或只需少量溶剂的固相微萃取技术(SPME)应运而生,其小巧便携,操作简单、快速,易于实现自动化等特点使之成为广泛应用的样品前处理技术。早期的研究大多采用商品化SPME装置,然而它的种类有限、价格昂贵、纤维易断、选择性不足,因此,近年来使用金属有机骨架化合物、共价有机骨架化合物、碳基材料、分子印迹聚合物、离子液体、导电聚合物等各种功能材料制备SPME涂层的技术越来越受到关注,在环境监测、食品分析及药物检测等方面应用广泛。然而这些SPME涂层材料在法庭科学领域的应用相对较少,考虑到SPME技术应用于犯罪现场样品原位高效提取的巨大潜力,该文对功能涂层材料进行了简要介绍,系统总结了基于功能材料的SPME技术在炸药、助燃剂、毒品、毒物、油漆、人体气味等分析中的应用,并指出了基于功能材料的SPME技术在法庭科学... 相似文献
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固相微萃取(SPME)近几年的发展 总被引:1,自引:0,他引:1
《分析试验室》2015,(5)
在化学分析中样品制备往往是整个分析方法的瓶颈,25多年前固相微萃取(SPME)的出现是样品制备领域极大的进步,大大促进了在现场和活体分析中的应用。本综述介绍近几年SPME的发展,值得介绍的是近年有许多适应于复杂基体的SPME涂层出现,可直接从复杂基体中萃取分析物。 相似文献
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《化学进展》2017,(9)
固相微萃取(SPME)是一种简便、快速、绿色的样品前处理方法,近年来引发了广泛关注。固相微萃取探针的萃取相对其萃取选择性和效率起着决定性作用,因此一系列物理化学性质优秀的新型固相微萃取涂层材料应运而生,被用于制备新型固相微萃取探针,以对不同样品基质中的有机小分子进行检测。本文概述了近年来新型SPME探针的研制所依托的新型材料,包括聚合物材料、碳材料、金属有机框架材料等,并重点阐述了相关材料的制备与固定方法、微观结构与萃取性能,以及所制备探针在环境分析、纺织品和皮革分析、食品分析等领域中的应用,并进一步对新型固相微萃取涂层今后的开发方向和应用前景进行了展望。 相似文献
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Priscilla Rocío-Bautista Idaira Pacheco-Fernández Jorge Pasán Verónica Pino 《Analytica chimica acta》2016
Solid-phase microextraction (SPME) is a powerful technique commonly used in sample preparation for extraction/preconcentration of analytes from a wide variety of samples. Among the trends in improving SPME applications, current investigations are focused on the development of novel coatings able to improve the extraction efficiency, sensitivity, and thermal and mechanical stability, within other properties, of current commercial SPME fibers. Metal-organic frameworks (MOFs) merit to be highlighted as promising sorbent materials in SPME schemes. MOFs are porous hybrid materials composed by metal ions and organic linkers, presenting the highest surface areas known, with ease synthesis and high tuneability, together with adequate chemical and thermal stability. For MOF based-SPME fibers, it results important to pretreat adequately the SPME supports to ensure the correct formation of the MOF onto the fiber or the attachment MOF-support. This, in turn, will increase the final stability of the fiber while generating uniform coatings. This review provides a critical overview of the current state of the use of MOFs as SPME coatings, not only highlighting the advantages of these materials versus commercial SPME coatings in terms of stability, selectivity, and sensitivity; but also insightfully describing the current methods to obtain reproducible MOF-based SPME coatings. 相似文献
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Dajana Vuckovic Yong Chen Craig Aurand Janusz Pawliszyn 《Analytica chimica acta》2009,638(2):175-3787
A new line of solid-phase microextraction (SPME) coatings suitable for use with liquid chromatography applications was recently developed to address the limitations of the currently available coatings. The proposed coatings were immobilized on the metal fiber core and consisted of a mixture of proprietary biocompatible binder and various types of coated silica (octadecyl, polar embedded and cyano) particles. The aim of this research was to perform in vitro assessment of these new SPME fibers in order to evaluate their suitability for drug analysis and in vivo SPME applications. The main parameters examined were extraction efficiency, solvent resistance, preconditioning, dependence of extraction kinetics on coating thickness, carryover, linear range and inter-fiber reproducibility. The performance of the proposed coatings was compared against commercial Carbowax-TPR (CW-TPR) coating, when applicable. The fibers were evaluated for the extraction of drugs of different classes (carbamazepine, propranolol, pseudoephedrine, ranitidine and diazepam) from plasma and urine. The analyses were performed using liquid chromatography-tandem mass spectrometry. The results show that the fibers perform very well for the extraction of biological fluids with no sample pre-treatment required and can also be used for in vivo sampling applications of flowing blood. A coating thickness of 45 μm was found to be a good compromise between extraction capacity and extraction kinetics. Due to the high extraction efficiency of these coatings, pre-equilibrium SPME with very short extraction times (2 min) can be employed to increase sample throughput. Inter-fiber reproducibility was ≤11% R.S.D. (n = 10) for model drugs examined in plasma, which is a significant improvement over polypyrrole coatings reported in literature, and permits single fiber use for in vivo applications. 相似文献
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Haberhauer-Troyer C Crnoja M Rosenberg E Grasserbauer M 《Fresenius' Journal of Analytical Chemistry》2000,366(4):329-331
The surfaces of commercially available polydimethylsiloxane (PDMS) and Carboxen-PDMS fibers for solid-phase microextraction (SPME) were investigated by optical and electron microscopy. Damage to the coating as well as contamination of new fibers and a highly variable number of pores in Carboxen-PDMS coatings were observed. Together with the contamination of the fibers during their use with metallic particles originating from the SPME fiber holder they are possible explanations for the problems encountered in the analysis of organolead, organotin and organosulfur compounds, such as artifact formation and low repeatability. 相似文献
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Solid-phase microextraction (SPME) has been popular as an environmentally friendly sample pretreatment technique to extract a very wide range of analytes. This is partly owing to the development of SPME coatings. One of the key factors affecting the extraction performances, such as the sensitivity, selectivity, and reproducibility, is the properties of the coatings on SPME fibers. This paper classifies the materials used as SPME coatings and introduces some common preparation techniques of SPME coating in detail, such as sol-gel technique, electrochemical polymerization technique, particle direct pasting technique, restricted access matrix SPME technique, and molecularly imprinted SPME technique. 相似文献
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Use of metal fibers in solid phase microextraction (SPME) can overcome the fragility drawback of conventional fused-silica ones. However, the surface modification of metal substrates is rather difficult, which largely prevents many mature traditional techniques, such as sol-gel and chemical bonding, being used in fabrication of SPME coating on metal-based fibers. This study demonstrates a protocol to resolve this problem by magnetron sputtering a firm Si interlayer on stainless steel fiber. The Si interlayer was easily modified active group, and attached with a multiwalled carbon nanotubes (MWCNTs) coating using the reported approach. The as-prepared MWCNTs/Si/stainless steel wire fiber not only preserved the excellent SPME behaviors of MWCNTs coatings, but also exhibited a number of advantages including high rigidity, long service life, and good stability at high temperature, in acid and alkali solutions. This new surface modification technique might provide a versatile approach to prepare sorbent coatings on unconfined substrates using traditional methods. 相似文献
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Pragst F 《Analytical and bioanalytical chemistry》2007,388(7):1393-1414
Solid-phase microextraction (SPME) is a miniaturized and solvent-free sample preparation technique for chromatographic–spectrometric
analysis by which the analytes are extracted from a gaseous or liquid sample by absorption in, or adsorption on, a thin polymer
coating fixed to the solid surface of a fiber, inside an injection needle or inside a capillary. In this paper, the present
state of practical performance and of applications of SPME to the analysis of blood, urine, oral fluid and hair in clinical
and forensic toxicology is reviewed. The commercial coatings for fibers or needles have not essentially changed for many years,
but there are interesting laboratory developments, such as conductive polypyrrole coatings for electrochemically controlled
SPME of anions or cations and coatings with restricted-access properties for direct extraction from whole blood or immunoaffinity
SPME. In-tube SPME uses segments of commercial gas chromatography (GC) capillaries for highly efficient extraction by repeated
aspiration–ejection cycles of the liquid sample. It can be easily automated in combination with liquid chromatography but,
as it is very sensitive to capillary plugging, it requires completely homogeneous liquid samples. In contrast, fiber-based
SPME has not yet been performed automatically in combination with high-performance liquid chromatography. The headspace extractions
on fibers or needles (solid-phase dynamic extraction) combined with GC methods are the most advantageous versions of SPME
because of very pure extracts and the availability of automatic samplers. Surprisingly, substances with quite high boiling
points, such as tricyclic antidepressants or phenothiazines, can be measured by headspace SPME from aqueous samples. The applicability
and sensitivity of SPME was essentially extended by in-sample or on-fiber derivatization. The different modes of SPME were
applied to analysis of solvents and inhalation narcotics, amphetamines, cocaine and metabolites, cannabinoids, methadone and
other opioids, fatty acid ethyl esters as alcohol markers, γ-hydroxybutyric acid, benzodiazepines, various other therapeutic drugs, pesticides, chemical warfare agents, cyanide, sulfide
and metal ions. In general, SPME is routinely used in optimized methods for specific analytes. However, it was shown that
it also has some capacity for a general screening by direct immersion into urine samples and for pesticides and other semivolatile
substance in the headspace mode. 相似文献
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C. Haberhauer-Troyer M. Crnoja E. Rosenberg M. Grasserbauer 《Analytical and bioanalytical chemistry》2000,366(4):329-331
The surfaces of commercially available polydimethylsiloxane (PDMS) and Carboxen-PDMS fibers for solid-phase microextraction
(SPME) were investigated by optical and electron microscopy. Damage to the coating as well as contamination of new fibers
and a highly variable number of pores in Carboxen-PDMS coatings were observed. Together with the contamination of the fibers
during their use with metallic particles originating from the SPME fiber holder they are possible explanations for the problems
encountered in the analysis of organolead, organotin and organosulfur compounds, such as artifact formation and low repeatability.
Received: 2 August 1999 / Revised: 5 October 1999 / Accepted: 6 October 1999 相似文献
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Fabrication of selective adsorption coatings plays a crucial role in solid-phase microextraction(SPME).Herein, new strategies were developed for the in-situ fabrication of novel cobalt-based carbonaceous coatings on the nickel-titanium alloy(Ni Ti) fiber substrate using ZIF-67 as a precursor and template through the chemical reaction of ZIF-67 with glucose, dopamine(DA) and melamine, respectively. The adsorption performance of the resulting coatings was evaluated using representative aromatic co... 相似文献
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The study on the performance of polyaniline as a fiber coating for solid-phase microextraction (SPME) purposes has been reported. Polyaniline coatings were directly electrodeposited on the surface of a stainless steel wire and applied for the extraction of some organochlorine pesticides (OCPs) from water samples. Analyses were performed using GC-electron capture detection (GC-ECD). The results obtained show that polyaniline fiber coating is suitable for the successful extraction of organochlorine compounds. This behavior is most probably due to the porous surface structure of polyaniline film, which provides large surface areas and allowed for high extraction efficiency. Experimental parameters such as adsorption and desorption conditions were studied and optimized. The optimized method has an acceptable linearity, with a concentration range of 1-5000 ng/L. Single fiber repeatability and fiber-to-fiber reproducibility were less than 12 and 17%, respectively. High environmental resistance and lower cost are among the advantages of polyaniline fibers over commercially available SPME fibers. The developed method was applied to the analysis of real water samples from Yangtse River and Tianmu Lake. 相似文献