固相微萃取新型涂层的制备和特性(英文)

 以聚甲基苯基乙烯基硅氧烷为主要成分 ,采用溶胶 凝胶技术和自由基引发交联反应的方法首次制备了一种固相微萃取新涂层 ,并与气相联用 ,分析了芳香族化合物 ,考察了它的萃取性能。结果表明 :该涂层提供了大的比表面积 ,可获得高的萃取效率。与相应的商用固相微萃取涂层相比 ,该涂层具有更好的灵敏度和选择性 ,且热稳定性好 ,使用寿命长。     

选择性固相微萃取涂层的研究进展

固相微萃取装置的核心部分是它的涂层,涂层的种类和厚度是影响分析灵敏度和选择性的最重要因素。具选择性的涂层可增强固相微萃取的分离能力,扩展它的应用范围。本文介绍了固相微萃取的类型,综述了近年来选择性固相微萃取涂层的研究进展,包括溶胶-凝胶涂层、限进介质涂层、分子印迹涂层等涂层的研制及应用。     

Ionic Liquid Based Ultrasound-Assisted Emulsification Microextraction for Preconcentration of Phenol Using Central Composite Design

In this work, phenol reacted with 4-aminoantipyrine (4-AAP) reagent in presence of potassium hexacyanoferrate(III) and then was extracted using ultrasound-assisted emulsification microextraction via 1-hexyl-3-methyl imidazolium hexafluorophosphate as an environmentally friendly solvent. Effects of the main experimental variables were investigated and optimized by central composite design. Under the optimum conditions (pH 9.5, 100 mg/L 4-AAP, 100 μL of ionic liquid as extraction solvent, 0.2 g/L K₃Fe(CN)₆ and 0.2 M NH₄Cl) the dynamic linear range, limit of detection and relative standard deviation were obtained as 0.2?25 μg/L, 0.07 μg/L and 2.6%, respectively. Finally, the applicability of the proposed ultrasoundassisted emulsification microextraction was examined and very good results were obtained. The results confirmed the applicability of the proposed method as a versatile, low cost and sensitive preconcentration method for determination of very low concentrations of phenol in aqueous solutions.     

聚硅氧烷富勒烯固相微萃取涂层的性能

高分子聚硅氧烷富勒烯首次被用作固相微萃取涂层材料,利用顶空固相萃取气相色谱法对该涂层进行了评价。与商用的聚二甲基硅氧烷相比,自制涂层在选择性、灵敏度、热稳定性、使用寿命及萃取量等方面的性能均优于商用聚二甲基硅氧烷。     

葫芦脲用作固相微萃取涂层新材料

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.     

溶胶-凝胶-硫化法制备硅橡胶吸附萃取搅拌棒

采用溶胶-凝胶-硫化法,以甲基乙烯基硅橡胶和乙烯基封端硅橡胶为原料制备了厚壁硅橡胶吸附萃取搅拌棒(stir bar for sorptive extraction,SBSE)。采用分段硫化和多阶程序升温老化防止涂层脱落和龟裂,一次涂渍涂层厚度约150~250μm,280℃下无流失,使用寿命可达150次。利用所制备涂层,结合自制热解析系统(thermal desorption system,TDS),建立了SBSE-TDS-CGC-FID测定水样中6种多环芳烃(polyaromatichydrocarbons,PAHs)的方法。方法的线性范围为0.3~1000μg/L,检出限为0.002~0.011μg/L,相对标准偏差在0.92%~6.14%之间。该方法能够满足欧盟2005/69/EC指令对多环芳烃低于10 mg/kg的检测要求。     

Microextraction Preconcentration of Chloroacetic Acids with the Flotation Separation of the Extract

Journal of Analytical Chemistry - A procedure is developed for liquid–liquid microextraction preconcentration of mono-, di-, and trichloroacetic acids (CAAs) with the flotation separation of...     

Novel Microporous Membrane/Solvent Microextraction for Preconcentration of Cinnamic Acid Derivatives in Rhizoma Typhonii

A novel microporous membrane/solvent microextraction (MPMSME) approach was developed in which a piece of microporous filter membrane was used as not only extraction solvent holder but also solid phase extraction unit. Subsequently, high-performance liquid chromatography with an UV detector was conducted. The wide exchange surface and very little organic solvent consumption made this sample pretreatment technology very interesting. The cinnamic acid derivatives were used as model analytes to evaluate the procedure. Parameters that affect the MPMSME such as type of extraction solvent, membrane area (or volumes of extraction solvent), aqueous phase pH, ionic strength, extraction stirring rate, extraction time, and sample volume were investigated and optimized. The enrichment factor (EF) of analyte was defined in MPMSME. Under the optimized conditions, the EFs of cinnamic acid derivatives were 43–144. Good linearities were obtained from 4 to 4,000 ng mL^?1 for all the analytes with regression coefficients of between 0.9956 and 0.9977; the limits of quantification were below 0.4 ng mL^?1, and satisfactory recoveries (93–106 %) and precisions (0.37–13 %) were also achieved. The experimental results showed that the method was simple, rapid, practical, and effective for preconcentration and determination of the cinnamic acid derivatives in rhizoma typhonii.     

固相微萃取中高分子涂层的研究

聚甲基乙烯基硅氧烷首次被用作固相微萃取（ＳＰＭＥ）装置的固相涂层,通过顶空固相微萃取气相色谱分析（ＨＳ－ＳＰＭＥ－ＧＣ）对使用聚甲基乙烯基硅氧烷固相涂层的ＳＰＭＥ装置进行了评价。对其使用厚度、温度及选择性进行了较深入的研究,找到了它的最佳使用条件和适用范围,并与商品化的ＳＰＭＥ涂层作了比较。对ＨＳ－ＳＰＭＥ－ＧＣ和ＨＳ－ＧＣ两种方法也作了比较,指出两者的适用范围不同。     

Capillary GC Determination of Amines in Aqueous Samples Using Sorptive Preconcentration on Polydimethylsiloxane and Polyacrylate Phases

The use of sorptive extraction/thermal desorption (SE/TD) for the enrichment of amines from aqueous samples was investigated. The amines were derivatized in situ in the water sample by pentafluorobenzoyl chloride and subsequently enriched onto the SE cartridge. Two SE/TD cartridges were used, a commercially available polydimethylsiloxane (PDMS) packed cartridge and a similar cartridge prepared with newly synthesized poly(butyl acrylate) (PBA). Blank profiles of PBA were not as good as those obtained from the PDMS phase. A complex chromatogram was obtained using mass spectrometric detection. Fortunately, the use of a nitrogen-phosphorus detector (NPD) resulted in clean blanks. The PBA phase showed superior performance for the enrichment of the polar amine derivatives from water samples compared to the PDMS material. Using a CGC-NPD set-up and only 1 mL samples, detection limits are in the sub-ppb range.     

Design of Sol-Gel Coating Media for Ink-Jet Printing

Image transfer and storage is rapidly becoming one of the most important technologies in the communication age. Ink-jet printing by which multicolor images are transferred onto paper and transparencies is a major branch of this technology. In this technology electronic image transfer capabilities are often limited by the shortcomings in the materials used. The coating designed to receive the ink determines the ink-dry time, edge acuity or patterns, color fidelity, as well as light and water fastness of the print. These in turn govern the speed, resolution and quality of the image transferred. Chemical, structural and process parameters involved in the design of a transparent, single layer sol-gel coating media for ink-jet printing are discussed. Design goals include quick drying of the print, water resistance, edge acuity without bleeding, UV protection of color dyes, and being printer nonspecific.     

自组装金纳米粒子涂层对环境水样中紫外线吸收剂的固相微萃取

以刻蚀不锈钢丝为基体,采用化学沉积法在表面沉积金纳米粒子(AuNPs),修饰一层1,8-辛二硫醇分子后,再自组装一层AuNPs,制备了高强度AuNPs涂层固相微萃取(SPME)纤维,并与HPLC联用,以常用紫外线吸收剂为例,评价了AuNPs-SPME纤维的萃取分离性能。当萃取时间为30 min、温度为55℃、搅拌速率为800 r/min,pH=7时,萃取效果最好。在优化的萃取条件下,所建立的Au NPs-SPME-HPLC法测定4种紫外吸收剂(2-羟基-4-甲氧基二苯甲酮、2-乙基己基-4-(N,N-二甲氨基)苯甲酸酯、2-乙基己基-4-甲氧基肉桂酸酯和2-乙基己基水杨酸)的线性范围为0.004~200μg/L,检出限为0.43~570 ng/L(S/N=3),相对标准偏差(RSD)在1.9%~4.2%(n=5)之间。河水、废水处理厂的废水以及雨水样品中紫外线吸收剂的加标回收率在77.9%~108%之间,RSD为3.1%~8.0%(n=5)。     

Comparative Study of Hyper-crosslinked Polymer-Solid Phase Microextraction and Stir Bar Fabric Phase Sorptive Extraction for Simultaneous Determination of Fluoroquinolones in Water

Chromatographia - Advancement of novel sorbent materials and efficient extraction mode is urgently needed for sorbent-phase microextraction techniques. Herein, two novel microextraction techniques,...     

A Review of Stir Bar Sorptive Extraction

Stir bar sorptive extraction (SBSE) is an extraction technique for enrichment of volatile and semi-volatile organic compounds from aqueous and gaseous media. After exposure to a sample, the stir bar, which is covered in a layer of a polysiloxane is subsequently removed and the sorbed compounds are then either thermally desorbed, and analysed by GC-MS or desorbed by means of a liquid, for improved selectivity or for interfacing to an LC system.The technique has been applied successfully to trace analysis in environmental, biomedical and food applications. Applications of SBSE to environmental, foodstuffs and pharmaceutical and biomedical samples are given.

     

有序介孔碳固相微萃取涂层测定水中氯苯类有机污染物

采用溶剂挥发自组装结合提拉法,在石墨纤维表面制备有序介孔碳(Ordered mesoporous cabon,OMC)涂层,并开展其对水中氯苯类有机污染物的固相微萃取(SPME)测定.扫描电镜(SEM)结果显示,制备的OMC涂层完整,与基体结合紧密,厚度约为7μm.透射电镜(TEM)、X射线衍射(XRD)和氮吸附脱附结果证实,OMC涂层具有规整二维六方特征,比表面积和孔容分别为369.7 m2/g和0.28 cm3/g.以氯苯类污染物为分析对象,采用顶空固相微萃取与氢火焰气相色谱联用法对OMC涂层的萃取性能进行全面的评价,优化萃取时间和温度、解吸时间、搅拌速率、离子强度及顶空体积等萃取条件,并与商品化涂层进行比对.结果表明,最佳萃取条件为:萃取时间30 min,萃取温度50℃,脱附时间2 min,盐浓度0.35 g/mL,顶空体积15 mL.在最佳萃取条件下,检出限在0.05～0.15 μg/L之间;在1～1000 μg/L线性范围内,线性关系良好;7次平行样测定的相对标准偏差为4.1％ ～6.4％.制备的OMC涂层的峰面积是商用聚二甲基硅氧烷/二乙烯基苯(Polydimethylsiloxane/divinylbenzene,PDMS/DVB)涂层的2倍,商用聚丙烯酸酯(Polyacrylate,PA)涂层的18倍.将此涂层应用于两种实际水样中,4种氯苯均未检出,添加浓度为20 μg/L时,样品回收率分别为99.4％～114.5％和92.3％～ 97.0％.     

水体中邻苯二甲酸酯类污染物在HLB柱净化条件优化的研究

采用全因子设计试验对水样中11种邻苯二甲酸酯类污染物在亲水-亲脂平衡介质固相萃取柱上的富集净化效果进行研究, 以邻苯二甲酸酯平均回收率为响应指标, 通过析因分析, 获得主因子及交叉因子效应, 并建立了由显著性因子及交叉因子表达的平均回收率方程. 通过对邻苯二甲酸酯平均回收率的响应曲面分析, 获得最优净化条件. 1.0 μg·L-1添加水平回收率为92% ～102%,50 μg·L-1添加水平回收率为93% ～101%;11种邻苯二甲酸酯的检出限为0.01 ～0.29 mg·L-1;线性范围在0.1 ～100 mg·L-1之间,相关性系数高于0.999 5,方法具有较高的回收率及测定精度.     

SPME涂层中硅烷化反应机理的研究

建立了SPME 涂层中硅烷化衍生化样品预处理方法,并用于葡萄酒中白黎芦醇的测定.SPME 硅烷化的反应动力学过程研究表明,涂层中硅烷化反应遵循假一级反应动力学,高温条件下硅烷化试剂会破坏极性聚丙烯酯(PA)涂层.     

Filters for the Preconcentration of Elements from Solutions

The main techniques for the preconcentration of elements on thin-layer filters are considered: sorption on filters with noncovalently immobilized reagents, bonded groups, and mechanically fixed sorbents and the extraction of elements on filters as poorly soluble and polymeric forms previously formed in solution. The matrix of the filters is cellulose, synthetic polymers of the linear and branched structures, synthetic fibers, reversed-phase silica gels, foamed polyurethanes, etc. The variation of the nature of the bonded group or the reagent introduced into the solution, the matrix material, and the technique for the immobilization of groups provides the preconcentration of elements with regard to the peculiarities of test materials and the method for the subsequent determination of elements. Methods for the determination of elements in different samples including preconcentration on filters are considered.     

An Electropolymerized Pyrrole‐based Coating for Stir Bar Sorptive Extraction of Btex from Water Followed by Gas Chromatography‐Mass Spectrometry

A stir bar sorptive extraction (SBSE) technique was developed by the use of polypyrrole (PPy) sorbent, electropolymerized on the surface of a rod, as a possible alternative to solid‐phase microextraction (SPME). Liquid desorption was subsequently employed to transfer the extracted analytes into the injection port of a gas chromatography‐mass spectrometry (GC‐MS). The PPy sorbent including polypyrrole‐dodecyl sulfate (PPy‐DS) was deposited on the surface of a stainless steel rod from the corresponding aqueous electrolyte by applying a constant deposition potential. The developed method was applied to the trace level extraction of BTEX (benzene, toluene, ethylbenzene, o,p‐xylene) from aqueous sample. Optimization of influential experimental conditions including the voltage of power supply, the time of PPy electrodeposition, the extraction temperature, the ionic strength and the extraction time were also investigated. The detection limits of the method under optimized conditions were in the range of 0.01–0.1 ng·mL?¹. The relative standard deviations (RSD) at a concentration level of 1 ng·mL?¹ were obtained between 8% and 13% (n=6). The calibration curves of BTEX showed linearity in the range of 0.03 to 600 ng·mL?¹. The proposed method was successfully applied to the extraction of some selected BTEX from river water samples and the relative recoveries were higher than 90% for all the analytes.