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PubMed2001

Solid phase microextraction.

Solid Phase Microextraction (SPME) uses a small volume of sorbent dispersed typically on the surface of small fibres, to isolate and concentrate analytes from sample matrix. After contact with sample, analytes are absorbed or adsorbed by the fibre phase (depending on the nature of the coating) until an equilibrium is reached in the system. The amount of an analyte extracted by the coating at equilibrium is determined by the magnitude of the partition coefficient of the analyte between the sample matrix and the coating material. After the extraction step, the fibres are transferred, with the help of a syringe-like handling device, to analytical instrument, for separation and quantitation of target analytes. This technique integrates sampling, extraction and sample introduction and is a simple way of facilitating on-site monitoring. Applications of this technique include environmental monitoring, industrial hygiene, process monitoring, clinical, forensic, food, flavour, fragrance and drug analyses, in laboratory and on-site analysis.

Chemistry Techniques, Analytical↗

PubMed1999

Determination of equilibrium constant of alkylbenzenes binding to bovine serum albumin by solid phase microextraction.

Solid phase microextraction (SPME) coupled with GC has been applied to study the binding properties between bovine serum albumin (BSA) and volatile organic compounds such as benzene, toluene, ethylbenzene, propylbenzene and butylbenzene. Their protein-ligand equilibrium constants have been determined. The measurement of free and bound ligand concentrations in the aqueous solution was based on the equilibrium among the analyte in the fiber coating (Cf), headspace (Ch) and aqueous solution (Cs). The work demonstrated that SPME is a simple and effective method in the study of protein binding to measure the freely dissolved analyte concentration as well as the equilibrium constant. The theoretical aspect of the SPME applied to the equilibrium constant measurement in two-phase (liquid sample-fiber coating) and three-phase (liquid sample-headspace-fiber coating) systems has been thoroughly discussed. The results demonstrated that the interpretation of the calibration data is crucial to the determination of freely dissolved analyte concentration and the equilibrium constant especially when the sample volume is small. The error in the experimental system is discussed. It is demonstrated in this study that for the three-phase system the amount of the analyte partitioned in the headspace could be ignored only in certain circumstances, where the Henry's law constant and the ratio between headspace volume and sample volume are sufficiently small.

Animals↗

PubMed2001

Air sampling and analysis of volatile organic compounds with solid phase microextraction.

Solid phase microextraction (SPME) presents many advantages over conventional analytical methods by combining sampling, preconcentration, and direct transfer of the analytes into a standard gas chromatograph (GC). Since its commercial introduction in the early 1990s, SPME has been successfully applied to the sampling and analysis of environmental samples. This paper presents an overview of the current methods for air sampling and analysis with SPME using both grab and time-weighted average (TWA) modes. Methods include total volatile organic compounds (TVOCs), formaldehyde, and several target volatile organic compounds (VOCs). Field sampling data obtained with these methods in indoor air were validated with conventional methods based on sorbent tubes. The advantages and challenges associated with SPME for air sampling are also discussed. SPME is accurate, fast, sensitive, versatile, and cost-efficient, and could serve as a powerful alternative to conventional methods used by the research, industrial, regulatory, and academic communities.

Air Pollutants↗

PubMed2006

Determination of sulfonamide antibiotics in wastewater: a comparison of solid phase microextraction and solid phase extraction methods.

In recent years, pharmaceutical and personal care products (PPCPs) have been detected in diverse environments (including groundwater, river water, and municipal wastewater). In order to evaluate their environmental impact, PPCPs must first be accurately determined. In this study, we focused on developing methods to accurately determine 10 sulfonamide antibiotics: sulfaguanidine, sulfacetamide, sulfadiazine, sulfathiazine, sulfapyridine, sulfamerazine, sulfamethazine, sulfamethoxazole, sulfadimethoxine, and sulfasalazine. While sulfonamides can easily be determined in pure water, wastewater influent and effluent collected from sewage treatment plants in Burlington and Toronto (Ontario) were found to generate confounding matrix effects. In an effort to overcome these matrix effects, we developed a solid phase microextraction (SPME) method to determine sulfonamides. Of the five different fiber assemblies investigated, the carbowax/divinylbenzene (CW/DVB) fiber produced the optimal response to sulfonamides. The SPME method was further optimized for sorption time (20min), solution salinity (10%, w/v, KCl), pH (4.5), and static desorption time (30min). When compared to solid phase extraction (SPE) using MCX cartridges, we observed that despite having higher MDLs and poorer sensitivity, SPME possessed the advantage of speed and reduced solvent usage. Most importantly, in contrast to SPE, when we applied the SPME method to fortified wastewater samples, we were generally able to accurately determine (i.e., recover) those sulfonamides that were present. Therefore, we conclude that SPME is a viable method for overcoming matrix effects in environmental samples.

Anti-Bacterial Agents↗

PubMed2000

Solid-phase microextraction and headspace solid-phase microextraction for the determination of high molecular-weight polycyclic aromatic hydrocarbons in water and soil samples.

The feasibility of direct-immersion (DI) solid-phase microextraction (SPME) and headspace (HS) SPME for the determination of high-ring polycyclic aromatic hydrocarbons (PAHs) (4- to 6-ring PAHs) in water and soil samples is studied. Three SPME fibers--100- and 30-microm polydimethylsiloxane (PDMS) and 85-microm polyacrylate (PA) fibers-are compared for the effective extraction of PAHs. Parameters affecting the sorption of PAHs into the fiber such as sampling time, sampling volume, and temperature are also evaluated. The extracted amounts of high-ring PAHs decrease with the decreasing of film thickness, and the 100-microm PDMS has the highest extraction efficiency than 85-microm PA and 30-microm PDMS fibers. Also, the extraction efficiency decreases with the increasing molecular weights of PAHs. Of the 10 high-ring PAHs, only fluoranthene and pyrene can reach equilibrium within 120 min at 25 degrees C for DI-SPME in a water sample. Increasing the temperature to 60 degrees C can increase the sensitivity of PAHs and shorten the equilibrium time. A 0.7- to 25-fold increase in peak area is obtained for DI-SPME when the working temperature is increased to 60 degrees C. For HS-SPME, the extraction efficiency of PAHs decrease when the headspace volume of the sampling system increases. All high-ring PAHs can be detected in a water sample by increasing the temperature to 80 degrees C. However, only 4- and 5-ring PAHs can be quantitated in a CRM soil sample when HS-SPME is used. The addition of a surfactant with high hydrophilic property can effectively enhance the sensitivity of high-ring PAHs. HS-SPME as well as DI-SPME with 100-microm PDMS or 85-microm PA fibers are shown to be suitable methods for analyzing high-ring PAHs in a water sample; however, this technique can only apply in a soil sample for PAHs having up to 5 rings.

Chromatography, Gas↗

PubMed2004

Enhanced extraction capacity and chemical noise reduction in solid-phase microextraction.

Solid-phase microextraction fibres with different lengths, coatings (polydimethylsiloxane, polyacrylate, Carbowax/divinylbenzene), film thicknesses, and mounting techniques were examined in combination with GC-MS with regard to their enhanced extraction capacities and fibre 'bleeding'. A series of phenols and halogenated aromatics with diverse physicochemical properties were investigated to characterize the effects of the enhanced extraction capacities of solid-phase microextraction fibres. Fibre extension was found to be effective for the microextraction of compounds with high log Kow values, whereas increasing both coating thickness and fibre length is most effective for the microextraction of more polar compounds such as phenols. Almost no bisphenol A was released when custom-made polydimethylsiloxane fibres were used, finally eliminating a drawback of endocrine disrupter analysis by solid-phase microextraction.

Journal Article↗

PubMed2003

Application of single-drop microextraction and comparison with solid-phase microextraction and solid-phase extraction for the determination of alpha- and beta-endosulfan in water samples by gas chromatography-electron-capture detection.

Water contamination due to the wide variety of pesticides used in agriculture practices is a global environmental pollution problem. The 98/83 European Directive requires the measurement of pesticides residues at a target concentration of 1.0 microg/l in surface water and 0.1 microg/l in drinking water. In order to reach the level of detection required, efficient extraction techniques are necessary. The application of a new extraction technique: single-drop microextraction (SDME), followed by gas chromatography with electron-capture detection, was assessed for determining alpha-endosulfan and beta-endosulfan in water samples. Experimental parameters which control the performance of SDME, such as selection of microextraction solvent and internal standard, optimization of organic drop volume, effects of sample stirring, temperature and salt addition, and sorption time profiles were studied. Once SDME was optimized, analytical parameters such as linearity, precision, detection and quantitation limits, plus matrix effects were evaluated. The SDME method was compared with solid-phase microextraction and solid-phase extraction with the aim of selecting the most appropriate method for a certain application.

Chromatography, Gas↗

PubMed1999

[Research of polymer coating in solid phase microextraction].

The solid phase microextraction (SPME) is a new extraction technique which has been developed rapidly in 1990s. It is a fast, simple, solventless and sensitive method for analyzing environmental samples. However, the solid phase materials of SPME are relatively limited. This paper presents the research work on a new type of solid phase, polymethylvinylsiloxane (PMVS), used in SPME. The phase with 1% vinyl content could be used in light curing. The PMVS solution was coated on the surface of silica fiber and was quickly cured by UV. Two fibers with 87 microns and 44 microns thick PMVS coatings were prepared. They were compared with commercial polymer coating SPME fibers through Headspace SPME Gas Chromatograph (HS-SPME-GC). The adsorption and desorption kinetics of PMVS were studied. The HS-SPME system was optimized and the differences between HS-SPME and HS were investigated as well. The results indicated that PMVS is efficient in extracting volatile and semi-volatile organic compounds and PMVS showed the high thermostability and easy-coating properties. The detection limit of SPME using 88 microns PMVS coating was about 1-5 micrograms/L.

English Abstract↗

PubMedDate not supplied

Characterisation of volatile organic compounds in stemwood using solid-phase microextraction.

Solid-phase microextraction (SPME), hydrodistillation and dynamic headspace combined with GC and GC-MS were applied and compared for the analysis of volatile organic compounds (VOCs) from coniferous wood. The SPME conditions (type of fibre, size of wood sample, temperature and exposure time) were optimised, and more than 100 VOCs and semi-volatile compounds extracted and identified from the sapwood and heartwood of Norway spruce (Picea abies). The total number of mono- and sesquiterpenes eluted and identified was similar for the SPME and hydrodistillation methods, but more semi-volatile compounds were released by hydrodistillation. By applying dynamic headspace at room temperature, it was possible to analyse only the most volatile compounds. The qualitative composition of VOCs was similar in spruce sapwood and heartwood, although Z-beta-ocimene occurred only in sapwood while fenchol was present only in heartwood. SPME sampling coupled with GC, applied here to the analysis of VOCs released from stemwood of firs for the first time, is a convenient, sensitive, fast, solvent-free and simple method for the determination of wood volatiles. The technique requires much smaller sample amounts compared with hydrodistillation, and the total amount of VOCs extracted and identified is higher than that obtained by hydrodistillation or dynamic headspace. The relative ratios of the main mono- and sesquiterpenes and -terpenoids were similar using the SPME-GC and hydrodistillation methods.

Organic Chemicals↗

PubMed2004

Development of fluorinated low temperature glassy carbon films for solid-phase microextraction.

Solid-phase microextraction (SPME) fibers with supported fluorinated glassy carbon are demonstrated for the first time. Oligo[1,3-dibutadiynylene-1,3-(tetrafluoro)phenylene] was synthesized and heated to temperatures that varied from 200 to 1000 degrees C to produce the fluorinated glassy carbon. The extent of graphitization of the glassy carbon increased as the processing temperature increased. The fluorinated glassy carbon selectively extracted monohalogenated benzenes from an aqueous solution when compared to the extraction of toluene. The selectivity increased in the order of phi-F < phi-Cl < phi-Br < phi-I. The selectivity for the halogenated compounds was greatest for the fluorinated glassy carbon phase processed at temperature below approximately 400 degrees C. Preliminary studies on the retention mechanism of the LTGC phase show that dispersive interactions are very important to the retention of halocarbons on the fluorinated LTGC. Finally, the selectivity of the fluorinated LTGC for halogenated compounds was compared to that of commercially available SPME fibers, such as poly(dimethylsiloxane), poly(dimethylsiloxane)/divinylbenzene (PDMS/DVB), and poly(dimethylsiloxane)/Carboxen (PDMS/Carboxen) fibers. As expected the fluorinated LTGC was more selectivity for the halogenated compounds. Interestingly the order of the increase in selectivity is opposite when comparing the fluorinated-LTGC and the three commercial fibers. A decrease in selectivity was observed going from fluorobenzene to iodobenzene using PDMS/DVB and PDMS/Carboxen fibers. While for the pure PDMS phase, there is a slight increase in selectivity from fluorobenzene to chlorobenzene but the remaining trend shows little change for bromobenzene and iodobenzene.

Carbon↗

PubMed2003

Physico-chemical approach to study organotin sorption-desorption during solid-phase microextraction.

Solid-phase microextraction (SPME) has become a real alternative to liquid-liquid extraction in the field of speciation of organometallic compounds. Despite the high performance of this preconcentration technique, matrix effects in natural samples can affect the analytical precision. In order to understand the origin of these disturbances and control the extraction step as best as possible, the sorption-desorption behaviour of organotins was studied. In the first part, this paper discusses the analytical problems encountered in the daily use of SPME due to the particular problems observed for phenyltins. The sorption profile of these compounds was modelled using experimental design methodology to confirm the first-order kinetics. Desorption of the compounds was also observed after a given time and could not be attributed to competition between organotin compounds. In the same way, butyl- and phenyltins were studied in the presence of humic substances, which acted as representatives of organic matter found in natural samples. These substances drastically decrease the extraction yields, but do not affect the sorption profile of butyl- and phenyltins.

Humic Substances↗

PubMed1997

Method optimization for the analysis of amphetamines in urine by solid-phase microextraction.

Solid-phase microextraction is under investigation in many laboratories for its usefulness in the analysis of an ever widening variety of compounds. As new classes of compounds are investigated and new challenges arise, the methods are adapted to accommodate them. Polar semivolatiles are increasingly under study as analytical targets, and difficulties with small partition coefficients and long equilibration times have been identified. Amphetamine and methamphetamine were selected as semivolatiles exhibiting these limitations, and methods to optimize their analyses were investigated. Amphetamines are frequently monitored in very complex matrixes. Headspace methods minimize interactions between the sample and the fiber and have proven useful for these analyses. Several areas of experimental design were considered in the process of method optimization. These included matrix modification by heating, stirring, methanol content, addition of salt, and pH buffering. It was found that these amphetamines could be reliably analyzed using modified sample conditions, with excellent sensitivity, limits of detection, and method linearity. Clinical urine samples were successfully analyzed and gave clean chromatograms with no interfering peaks. Finally, the method developed was found to be useful for the analysis of narcotic analgesics. In the future, it is hoped that the method can be used to develop a general screen for a wide range of drugs of abuse.

Amphetamines↗

PubMed1997

Determination of methylcyclopentadienyl manganese tricarbonyl in beverages by solid-phase microextraction.

Solid-phase microextraction (SPME) was used to determine methylcyclopentadienyl manganese tricarbonyl (MMT), a gasoline antiknock additive, in beverages. MMT levels in beverages exposed to gasoline vapours for 1 h ranged from 0.62 to 2.84 ng/ml and continued to increase up to 16 h. A capillary gas chromatograph (GC) was coupled to an atomic absorption spectrometer (AAS) for element specific detection. The limit of detection was 4 pg MMT. Method limits of detection for MMT varied from 0.4 pg to 260 pg/ml depending on the beverage.

Beverages↗

PubMed2002

Optimum methamphetamine profiling with sample preparation by solid-phase microextraction.

Solid-phase microextraction (SPME) is a relatively new technique in which a small, polymer-coated fiber is employed to extract volatile and semivolatile organic compounds from the sealed headspace above a questioned sample. SPME, coupled with gas chromatography/mass spectrometry (GC/MS), was used to characterize impurities in illicit methamphetamine samples. Trace impurities present in a specimen were tentatively identified using mass-spectral databases and included 1,2-dimethyl-3-phenyl-aziridine (indicating synthesis via a halogenated ephedrine intermediate), ethyl vanillin (a flavoring compound), and caffeine (a stimulant used as cutting agent). The types and numbers of organic compounds sampled by SPME were compared with those collected by various solvent extraction protocols. In addition to unambiguously confirming the presence of methamphetamine, SPME-GC/MS analyses detected approximately 30 more organic analytes than were found by GC/MS following the ethyl acetate extraction method adopted by the United Nations International Drug Control Programme. SPME-GC/MS is a superior method for generating material "fingerprint" profiles in methamphetamine samples. The detection and characterization of increased points of comparison in drug samples provide more detailed chemical signatures for both intelligence and operational information.

Journal Article↗

PubMed2002

[New technologies of solid-phase microextraction].

Solid-phase microextraction (SPME) is a technology with functions of sampling, extraction and concentration based on adsorption/absorption-desorption equilibrium between coating and sample. The recent development of SPME is reviewed. Studies on the in-tube-SPME technology, novel extraction probes and its coupling with other analytical technologies are summarized.

Adsorption↗

PubMed2004

[Developments in preparation and experimental method of solid phase microextraction fibers].

Solid phase microextraction (SPME) is a simple and effective adsorption and desorption technique, which concentrates volatile or nonvolatile compounds from liquid samples or headspace of samples. SPME is compatible with analyte separation and detection by gas chromatography, high performance liquid chromatography, and other instrumental methods. It can provide many advantages, such as wide linear scale, low solvent and sample consumption, short analytical times, low detection limits, simple apparatus, and so on. The theory of SPME is introduced, which includes equilibrium theory and non-equilibrium theory. The novel development of fiber preparation methods and relative experimental techniques are discussed. In addition to commercial fiber preparation, different newly developed fabrication techniques, such as sol-gel, electronic deposition, carbon-base adsorption, high-temperature epoxy immobilization, are presented. Effects of extraction modes, selection of fiber coating, optimization of operating conditions, method sensitivity and precision, and systematical automation, are taken into considerations in the analytical process of SPME. A simple perspective of SPME is proposed at last.

Chromatography, Gas↗

PubMedDate not supplied

Factors affecting multiresidue determination of priority herbicides when using solid-phase microextraction.

A solid-phase microextraction (SPME) procedure was developed for the determination of 10 selected organonitrogen herbicides (s-ethyl dibropylthiocarbamate [EPTC], molinate, propachlor, trifluralin, simazine, atrazine, propazine, terbuthylazine, alachlor, and prometryn) and was tested with various natural waters. Gas chromatography coupled with flame thermionic and mass spectrometric detection was used for quantitation. For this purpose, polydimethylsiloxane and polyacrylate fibers were used and the factors affecting the SPME process such as pH, ionic strength, methanol content, memory effect, stirring rate, and adsorption-time profile were investigated and optimized. By using spiked liquid chromatography water, optimal factors were determined to be 25% salt, <0.5% methanol, stirring rate of 960 rpm, pH 4, and an equilibrium time of 30 min. These conditions were used in further studies of the fibers and in analysis of natural water samples. The method was applied to spiked natural waters such as ground water, sea water, lake water, and river water at a concentration range of 0.5-10 microg/L. Limits of detection ranged from 5 to 90 ng/L, and precision ranged from 5 to 15% (as relative standard deviation), depending on the pesticide, fiber, and detector used. The recoveries of herbicides were 70.2-118.4%, and the average r2 values of the calibration curves were >0.99 for all analytes. The results demonstrate the suitability of the SPME method to determine these organonitrogen herbicides in various natural waters. River water samples originating from the Epirus region (Northwestern Greece) were analyzed to verify the performance of the optimized method by comparing the results obtained by SPME with those obtained by using conventional solid-phase extraction of the selected herbicides.

Calibration↗

PubMed2000

Gas chromatography/ion trap tandem mass spectrometry for the analysis of halobenzenes in soils by solid-phase microextraction.

Headspace solid-phase microextraction combined with gas chromatography/ion trap tandem mass spectrometry (HS-SPME/GC/ITMS/MS) was used for the analysis of 12 halobenzenes from soil samples. For MS/MS optimisation, the experiments were performed by precursor ion selection and software controlled operations. Collision-induced dissociation (CID) can be achieved by two different approaches, resonant and non-resonant excitation modes. Different results were obtained using the two approaches, and the resonant excitation mode was chosen as the best for all halobenzenes. Parameters such as the CID excitation amplitude, excitation RF storage level and CID bandwidth frequency were optimised to maximise the formation of halobenzene product ions. A 100-microm polydimethylsiloxane fibre was used for the isolation and preconcentration of the analytes. The HS-SPME/GC/ITMS/MS method was applied to the analysis of halobenzenes in an agricultural soil sample. The halobenzenes were quantified by standard addition, which led to good reproducibility (RSD between 4.7 and 9.2%) and detection limits in the low pg/g range. The method was validated by comparing the results with those obtained in a European inter-laboratory exercise.

Benzene Derivatives↗