Recovery of Cadmium(II) Ions with a Sulfur-Containing Carbon Sorbent

The sorptive properties of a sulfur-containing sorbent, selective with respect to cadmium(II) ions in extraction from aqueous solutions, including process solutions, were studied.     

Sol–gel‐graphene‐based fabric‐phase sorptive extraction for cow and human breast milk sample cleanup for screening bisphenol A and residual dental restorative material before analysis by HPLC with diode array detection

Fabric‐phase sorptive extraction has already been recognized as a simple and green alternative to the conventional sorbent‐based sorptive microextraction techniques, using hybrid organic–inorganic sorbent coatings chemically bonded to a flexible fabric surface. Herein, we have investigated the synergistic combination of the advanced material properties offered by sol–gel graphene sorbent and the simplicity of Fabric phase sorptive extraction approach in selectively extracting bisphenol A and residual monomers including bisphenol A glycerolatedimethacrylate, urethane dimethacrylate, and triethylene glycol dimethacrylate derived dental restorative materials from cow and human breast milk samples. Different coatings were evaluated. Final method development employed sol–gel graphene coated media. The main experimental parameters influencing extraction of the compounds, such as sorbent chemistry used, sample loading conditions, elution solvent, sorption stirring time, elution time, impact of protein precipitation, amount of sample, and matrix effect, were investigated and optimized. Absolute recovery values from standard solutions were 50% for bisphenol A, 78% for T triethylene glycol dimethacrylate, 110% for urethane dimethacrylate, and 103% for bisphenol A glycerolatedimethacrylate, while respective absolute recovery values from milk were 30, 52, 104, and 42%. Method validation was performed according to European Decision 657/2002/EC in terms of selectivity, sensitivity, linearity, accuracy, and precision.     

Sulfonated polyvinyl chloride fibers for cation-exchange microextraction

Polyvinyl chloride (PVC) fiber was derivatized by concentrated sulfuric acid to yield sulfonated PVC (PVC-SO₃H). The PVC-SO₃H fiber had dual properties as a sorbent, based on cation-exchange and hydrophobicity. In the present study, the novel fiber was used directly as an individual device for extraction purposes in the cation-exchange microextraction of anaesthetics, followed by high-performance liquid chromatography-UV analysis. The results demonstrated that this PVC-SO₃H fiber-based microextraction afforded convenient operation and cost-effective application to basic analytes. The limits of detection for four anaesthetics ranged from 1.2 to 6.0 ng/mL. No carryover (because of its disposable usage), and no loss of sorbent phase (which normally occurs in stir-bar sorptive extraction) during extraction were observed.     

A new rotating-disk sorptive extraction mode,with a copolymer of divinylbenzene and N-vinylpyrrolidone trapped in the cavity of the disk,used for determination of florfenicol residues in porcine plasma

A novel extraction approach was developed based on rotating-disk sorptive extraction (RDSE). In this approach the rotating-disk extraction device consists of a Teflon disk, with a cavity that is loaded with a commercial sorbent phase selected according to the polarity of the analyte. To avoid leakage of the sorbent, the cavity is covered with a fiberglass filter and sealed with a Teflon ring. The proposed novel analytical RDSE technique was used in this study to determine florfenicol levels in plasma as a model analyte, or sample system, to describe the pharmacokinetics of a veterinary formulation. The sorbent used for this application was the copolymer of divinylbenzene and N-vinylpyrrolidone (Oasis HLB), which was selected because the florfenicol molecule contains both hydrophilic and lipophilic moieties. After the extraction, final determination of the analyte was performed by HPLC–DAD. Calibration plots and other analytical features were obtained after 90 min of extraction. The calibration plot was linear over the interval 0.4–16 μg mL^?1 (n?=?6), with R ²?=?0.9999. Recovery and repeatability were determined using a blank plasma sample spiked with 4.8 μg mL^?1 florfenicol. A recovery of 91.5 %, with a relative standard deviation (RSD) of 8.8 %, was obtained when the extraction was evaluated using six different rotating-disk devices. Precision was also assessed, using the same disk (containing the same sorbent phase) for eight aliquots of the same sample. The RSD under these conditions was 10.2 %, clearly indicating that the sorptive phase could possibly be re-used. Accordingly, RDSE is a suitable sample preparation alternative to liquid–liquid extraction (LLE), solid-phase extraction (SPE), and stir-bar sorptive extraction (SBSE).     

Headspace sampling of the volatile fraction of vegetable matrices

The evolution of vapour phase sampling of the volatile fraction of vegetable matrices, or of products directly related to them, over the period 1996-2007 is reviewed. High concentration capacity headspace (HCC-HS) and dynamic headspace (D-HS) techniques, that is headspace sampling approaches where the analytes in the vapour phase are concentrated into a sorbent, an adsorbent or a solvent, are considered. Advantages, disadvantages and applications to the vegetable field of several successful techniques based on these approaches are critically presented, including in-tube sorptive extraction (INCAT, HS-SPDE), headspace sorptive extraction (HSSE), solid-phase aroma concentrate extraction (SPACE), large surface area HCC-HS sampling (MESI, MME, HS-STE), headspace liquid-phase microextraction (HS-LPME) and dynamic headspace samplings (D-HS). The developments necessary to overcome some of the limits of the above approaches and techniques are also discussed in view of their application to new fields.     

Preparation,characterization and evaluation of a hybrid polymeric coating with sorbent properties

A hybrid polymeric coating (PDMS–CNPrTEOS) with sorbent properties was prepared by the sol–gel method from hydroxyl-terminated poly(dimethylsiloxane) (OH-PDMS), and cyanopropyltriethoxysilane (CNPrTEOS) as an inorganic precursor, using trifluoroacetic acid (TFA) as a catalyst. A coating with the sol–gel solution was prepared on glass plates using the dip-coating method and subsequently characterized. Characterization by FTIR shows that cyano groups are present on the surface coating and contact angle tests show that the coating presents hydrophilic characteristics. The organic–inorganic polymer was stable up to 400 °C with a weight loss of 8 wt % and showed good stability after immersion for 60 min in vortex and 45 min in ultrasonic bath, in various solvents: water, methanol (MeOH), acetone, isooctane, ethyl acetate (AcOEt) and acetonitrile (ACN), and solutions at different pH (1–12) for 48 h (h). The PDMS–CNPrTEOS hybrid polymer was evaluated and was found to have the ability to extract simultaneously furanic compounds in aqueous solution when it is employed as a sorbent for stir bar sorptive extraction (SBSE).     

Recent developments in solid-phase microextraction for on-site sampling and sample preparation

On-site sampling and sample preparation favor portable, solventless or even solvent-free techniques. Solid-phase microextraction (SPME) has these advantages. This review focuses on developments between 2007 and early 2011 in microextraction techniques for on-site sampling and sample preparation, including fiber SPME, stir-bar sorptive extraction (SBSE), thin-film microextraction (TFME) and different types of in-needle SPME. The major trends in on-site applications of SPME appear to be fiber and thin-film SPME, microextraction by packed sorbent (MEPS) and the sorbent-packed needle-trap device (NTD). We discuss and compare several aspects of these types of SPME in on-site applications. We also describe sorbent phases for SPME that benefit on-site applications. Finally, we provide a perspective on SPME-based techniques for on-site applications.     

GC-MS法测定大气样品的前处理研究--碳化纤维树脂捕集大气中痕量多环芳烃

研究了碳化纤维树脂吸附载体采集大气中多环芳烃(PAHs)的性能、样品前处理条件和毛细管气相色谱－质谱联用仪检测PAHs的,地具有代表性的多个采样点进行了实地采样、分析,证明碳化纤维树脂吸附载体是一种性能独特的固相吸附剂,建立的样品前处理方法可行,分析数据可靠,可用于大气中PAHs的检测。     

Determination of osmium by the sorption-X-ray fluorescence technique

Sorption of osmium(IV, VI) on complexing sorbents POLYORGS XXIV, POLYORGS 32 M, and POLYORGS 32 V and on the PVA-PGMA-PEPA sorbent from alkaline and hydrochloric acid solutions is studied. It is demonstrated that equilibrium in systems under study is attained within 40 min for the POLYORGS XXIV sorbent and within 2.5 h for the POLYORGS 32 V sorbent and that the sorbents exhibit a sufficiently high sorptive capacity with respect to osmium: from 3.4 to 8 mg of Os(VI) in alkaline solutions and 2.2 mg of Os(IV) in acidic solutions. Optimal conditions of analysis of a concentrate on an EDX-771 energy-dispersive X-ray fluorescence spectrometer are revealed and, on this basis, a sorption-X-ray fluorescence method that provides the determination of osmium in a wide concentration range with the detection limit down to 10^-6% is developed.     

Determination of the sorption characteristics of glauconite during extraction of a pharmaceutical from an aqueous medium

A technique for preparing enriched glauconite on the basis of a natural mineral from the Beloozyorskoe field of Saratov oblast has been developed. The results of a study of the chemical composition, surface structure, and certain physicochemical properties of the samples of the sorbent are presented. The sorption of ambroxol hydrochloride ions from aqueous solutions has been studied using natural and enriched glauconite. The sorption isotherms, are approximated by the Langmuir equation, have been obtained, and the values of the maximum sorptive capacities have been calculated. Based on the obtained data, conclusions have been drawn on using the studied natural mineral sorbents to extract the above-mentioned substance from aqueous solutions.     

CARBONIZED FIBROUS RESIN AS A NEW SORBENT FOR SAMPLING POLYCYCLIC AROMATIC HYDROCARBONS （PAHS）IN AMBIENT AIR

A new sampling method of ambient air analysis using carbonized fibrous resin as a sorbent for polycyclic aromatic hydrocarbons(PAHs) was reported.The physical and chemical properties of the carbonized fibrous resins were measured.The sample pretreatment with ultrasonic extraction and subsequent clean-up elution through a silica gel column was optimized.The suitable ultrasonic extraction conditions were selected as follows:resin weight was 1.5g,ultrasonic extraction time 20min,volume of extraction solvent 100 ml and extraction operation times 2-3.The concentrated extractable organic matter was submitted to next step of clean-up procedure of adsorption chromatography on silica gel column/n-hexane and a mixture of dichloromethene:n-hexane solution 2:3(v/v).The PAHs fractions in the real samples from Changzhou,China were particularly analyzed using GC-MS data system and the data of mass spectra,retention times and scan numbers of the real samples were compared with that of the standards of 16 PAHs listed by the US EPA as “priority pollutants” of the environment. The pretreatment of samples of ambient air with carbonized fibrous resin as a sorbent for PAHs is proved to be reliable and might be used for the procedure of the determination of PAHs in atmospheric environment.     

The role of graphene‐based sorbents in modern sample preparation techniques

The application of graphene‐based sorbents in sample preparation techniques has increased significantly since 2011. These materials have good physicochemical properties to be used as sorbent and have shown excellent results in different sample preparation techniques. Graphene and its precursor graphene oxide have been considered to be good candidates to improve the extraction and concentration of different classes of target compounds (e.g., parabens, polycyclic aromatic hydrocarbon, pyrethroids, triazines, and so on) present in complex matrices. Its applications have been employed during the analysis of different matrices (e.g., environmental, biological and food). In this review, we highlight the most important characteristics of graphene‐based material, their properties, synthesis routes, and the most important applications in both off‐line and on‐line sample preparation techniques. The discussion of the off‐line approaches includes methods derived from conventional solid‐phase extraction focusing on the miniaturized magnetic and dispersive modes. The modes of microextraction techniques called stir bar sorptive extraction, solid phase microextraction, and microextraction by packed sorbent are discussed. The on‐line approaches focus on the use of graphene‐based material mainly in on‐line solid phase extraction, its variation called in‐tube solid‐phase microextraction, and on‐line microdialysis systems.     

Cellulose fibrous sorbents with conformationally flexible aminocarboxylic groups for preconcentration of metals

New cellulose fibrous sorbents, containing a diethylenetriamine tetraacetate groups, are proposed for the preconcentration of heavy metals. Quantitative extraction of heavy metals from river and sea water is achieved in a wide pH range (3–8) at a high solution flow rate (up to 100–150 volumes of sorbent per minute). Quantitative desorption of metals is achieved with a very small volume of the acid.     

Fast extraction of amphenicols residues from raw milk using novel fabric phase sorptive extraction followed by high-performance liquid chromatography-diode array detection

A simple, sensitive, reliable, and fast analytical method was developed for the simultaneous determination of amphenicols residues in raw milk by combining fabric phase sorptive extraction (FPSE) and high-performance liquid chromatography-diode array detection. FPSE, a new generation green sample preparation technique, efficiently incorporates the advanced and tunable material properties of sol–gel derived microextraction sorbents with the rich surface chemistry of a cellulose fabric substrate, resulting in a flexible, highly sensitive, and fast microextraction device capable of extracting target analytes directly from complicated sample matrices. Due to the strong chemical bonding between the sol–gel sorbent and substrate, the microextraction device demonstrates a very high chemical and solvent stability. Therefore, any organic solvent/solvent mixture can be used as the eluent/back-extraction solvent.     

Sequestration of agrochemicals from aqueous media using cross-linked chitosan-based sorbents

The sorption properties are reported for chitosan and its cross-linked forms (chitosan-glutaraldehyde; CG) with some model agrochemical sorbates [pentachlorophenol (PCP), 2,4-dichlorophenol (2,4-DCP) and 2,4-dichlorophenoxy acetic acid (2,4-D), dicamba and carbofuran]. The CG cross-linked materials were prepared at variable C:G monomer mole ratios: 1:0.5 (CG1), 1:1 (CG2), (CG3). The sorbents were characterized using diffuse reflectance infrared Fourier transform spectroscopy, thermogravimetric analysis and a dye sorption method using phenolphthalein. The sorption studies were carried out in aqueous solution at pH 9 except for dicamba and carbofuran (pH 7). The isotherm results were evaluated by the Sips, Freundlich, and Langmuir models. The Sips model provided the “best-fit” results where the sorption capacity increased as the cross-linker content of the CG materials increased. The relative uptake for chitosan and its cross-linked forms adopted the following order: PCP > 2,4-DCP > 2,4-D. In the case of dicamba and carbofuran, the former had a higher sorptive uptake. The variable uptake of the sorbates were attributed to their relative lipophilicity where the main driving force of these solid-solution systems relates to hydrophobic effects, in accordance with the tunable physicochemical properties of the chitosan sorbent materials.     

Electrospun nanofibers as sorbent material for solid phase extraction

Electrospinning has emerged as the most versatile technique for nanofiber fabrication. Owing to their large surface area to volume ratio, electrospun nanofibers have the potential to serve as a good sorbent material for solid phase extraction (SPE) based techniques. The ability to incorporate a variety of functionalities prior or post-electrospinning presents a platform to tune the sorbents for specific applications. It is the aim of this contribution to highlight some of the recent developments that harness the great potential of electrospun nanofibers as sorbents for SPE. The review discusses the various ways in which the electrospinning technique addresses two important parameters for sorbent material, which are sorptive capacity and selectivity. It concludes by presenting and discussing the potential for development of SPE format technology and configurations based on electrospun nanofibers.     

Sample preparation for the analysis of volatile organic compounds in air and water matrices

This review summarizes literature data from the past 5 years on new developments and/or applications of sample preparation methods for analysis of volatile organic compounds (VOC), mainly in air and water matrices. Novel trends in the optimization and application of well-established airborne VOC enrichment techniques are discussed, like the implementation of advanced cooling systems in cryogenic trapping and miniaturization in adsorptive enrichment techniques. Next, focus is put on current tendencies in integrated sampling-extraction-sample introduction methods such as solid phase microextraction (SPME) and novel in-needle trapping devices. Particular attention is paid to emerging membrane extraction techniques such as membrane inlet mass spectrometry (MIMS) and membrane extraction with a sorbent interface (MESI). For VOC enrichment out of water, recent evolutions in direct aqueous injection (DAI) and liquid-liquid extraction (LLE) are highlighted, with main focus on miniaturized solvent extraction methods such as single drop microextraction (SDME) and liquid phase microextraction (LPME). Next, solvent-free sorptive enrichment receives major attention, with particular interest for innovative techniques such as stir bar sorptive extraction (SBSE) and solid phase dynamic extraction (SPDE). Finally, recent trends in membrane extraction are reviewed. Applications in both immersion and headspace mode are discussed.     

Adsorption of Fire Retardant from Dilute Aqueous Solutions onto Viscose Fiber

The adsorption isotherms of the product of transesterification of dimethyl methylphosphonate (ZG-2), used as fire retardant, from dilute solutions on viscose fiber were determined experimentally at various temperatures. The parameters of pore structure of the fibrous sorbent were estimated using the general equation of the theory of volume filling of micropores.     

Trace determination of parabens in cosmetics and personal care products using fabric‐phase sorptive extraction and high‐performance liquid chromatography with UV detection

A simple, fast, and sensitive analytical protocol using fabric‐phase sorptive extraction followed by high performance liquid chromatography with ultraviolet detection has been developed and validated for the extraction of five parabens including methylparaben, ethylparaben, propylparaben, butylparaben, and benzylparaben. In the present work, sol‐gel polyethylene glycol coated fabric‐phase sorptive extraction membrane is used for the preconcentration of parabens (polar) from complex matrices. The use of fabric‐phase sorptive extraction membrane provides a high surface area which offers high sorbent loading, shortened equilibrium time, and overall decrease in the sample preparation time. Various factors affecting the performance of fabric‐phase sorptive extraction, including extraction time, eluting solvent, elution time, and pH of the sample matrix, were optimized. Separation was performed using a mobile phase consisting of water:acetonitrile (63:37; v/v) at an isocratic elution mode at a flow rate of 0.9 mL/min with wavelength at 254 nm. The calibration curves of the target analytes were prepared with good correlation coefficient values (r² > 0.9955). The limit of detection values range from 0.252 to 0.580 ng/mL. Finally, the method was successfully applied to various cosmetics and personal care product samples such as rose water, deodorant, hair serum, and cream with extraction recoveries ranged between 88 and 122% with relative standard deviation <5%.     

Rotating disk sorbent extraction for pre-concentration of chromogenic organic compounds and direct determination by solid phase spectrophotometry

A novel and very simple microextraction approach for pre-concentration and direct solid phase spectrophotometric measurement has been developed for the determination of chromogenic analytes. The model analyte to assess this approach was the chromophore malachite green (MG). The analyte was extracted from water samples onto a small rotating disk made of Teflon containing a sorbent phase of polydimethylsiloxane (PDMS) on one of its surfaces. We refer to the extraction procedure as rotating disk sorptive extraction (RDSE). After extraction, the sorbent phase with the concentrated analyte was separated from the Teflon disk and used directly for MG determination by solid phase spectrophotometry at 624 nm, without the necessity of a desorption step. Chemical and extraction variables such as concentration of sodium sulfate, pH, disk rotational velocity, extraction time, and temperature were studied in order to establish the best conditions for extraction. Under optimum conditions, the extraction of MG was carried out in 18 min and 90 min, for sample volumes of 100mL or 1000 mL, respectively. The detection limit, based on three times the standard deviation of the blank phase (3σ(b)), was 1.4 μg L?1 and the repeatability, expressed as relative standard deviation (RSD), for 20 μg L?1 MG was 8.1%. This study also applied the method to real samples, obtaining quantitative recovery (mean recovery of 99.3%). The PDMS phases could be reused after desorbing the MG into methanol for 3h. Replacement of the PDMS film onto the disk is very easy and low cost.