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Results for “Solid Phase Microextraction”

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At least 217 records · Page 12Linked to original sources

PubMed2000

Solid-phase microextraction method development for headspace analysis of volatile flavor compounds.

Solid-phase microextraction (SPME) fibers were evaluated for their ability to adsorb volatile flavor compounds under various conditions with coffee and aqueous flavored solutions. Experiments comparing different fibers showed that poly(dimethylsiloxane)/divinylbenzene had the highest overall sensitivity. Carboxen/poly(dimethylsiloxane) was the most sensitive to small molecules and acids. As the concentrations of compounds increased, the quantitative linear range was exceeded as shown by competition effects with 2-isobutyl-3-methoxypyrazine at concentrations above 1 ppm. A method based on a short-time sampling of the headspace (1 min) was shown to better represent the equilibrium headspace concentration. Analysis of coffee brew with a 1-min headspace adsorption time was verified to be within the linear range for most compounds and thus appropriate for relative headspace quantification. Absolute quantification of volatiles, using isotope dilution assays (IDA), is not subject to biases caused by excess compound concentrations or complex matrices. The degradation of coffee aroma volatiles during storage was followed by relative headspace measurements and absolute quantifications. Both methods gave similar values for 3-methylbutanal, 4-ethylguaiacol, and 2,3-pentanedione. Acetic acid, however, gave higher values during storage upon relative headspace measurements due to concurrent pH decreases that were not seen with IDA.

Chromatography, Gas↗

PubMed2000

Quantitative analysis of acetates in cigarette tobacco using solid-phase microextraction and gas chromatography-mass spectrometry.

A method incorporating solid-phase microextraction (SPME) and gas chromatography-mass spectrometry for the headspace analysis of selected volatile organic compounds present in cigarette tobacco is developed and evaluated. Quantitative information on methyl, ethyl, n-propyl, isopropyl, isopropenyl, vinyl, and butyl acetates present in 29 different flavor variants (full, light, and ultra-light) of the top ten selling brands in the United States is presented. The concentrations of the various acetate analytes range from the low nanaogram to microgram levels per cigarette. Clear differences are observed in the concentrations of various acetates when comparing the levels in brands from different manufacturers. The SPME technique provides a method that allows high sample throughput, requires little sample preparation, and yields useful analytical information. High precision is obtained on multiple measurements of cigarettes from an individual pack, but lower precision levels are observed in general when comparing results obtained on the analysis of cigarettes from different packs of the same brand. The higher pack-to-pack variations may be due in part to product aging with a proportionate amount of evaporative loss of the relatively volatile acetates.

Acetates↗

PubMed2003

Determination of trace RA by capillary electrophoresis-solid-phase microextraction with direct UV detection.

A new method of offline solid-phase microextraction coupled with capillary electrophoresis (CE) [in an uncoated capillary using borax and boric acid in acetonitrile-water (40:60) as the running buffer] with UV detection at 254 nm is presented and used for direct determination of trace biomedically important retinoic acid (RA) without any derivation. As low as 138 ng/mL RA in aqueous solution can be determined using CE with UV detection with a concentration factor of 19.6 times.

Electrophoresis, Capillary↗

PubMed1999

[The study of carbonaceous adsorbent for solid-phase microextraction and the comparison with commercial device].

The parameters governing solid-phase microextraction have been investigated, and the development of carbonaceous adsorbent for SPME is presented because it is durable and inexpensive. The time profile curves were determined for several organic pesticides having a wide range of water solubilities and the effect of salt was also investigated. The method of SPME-GC-ECD to analyse trace level of the organic pesticide in water is established by the determination of optimum parameters. The comparison with commercial SPME device shows that the carbonaceous adsorbent having been treated with physical or chemical method for SPME can get lower limits of detection than polyacrylate and polydimethylsiloxane, although there are still some work to be done to improve its precision. The results shows that this new SPME device has great application potential.

Acrylic Resins↗

PubMed1998

Solid-phase microextraction for quantitative analysis of organophosphorus pesticides in environmental water samples.

Solid-phase microextraction (SPME) is a relatively new technique that appears as a convenient and efficient extraction method in contrast with more complex techniques used for pesticide residue analysis based on liquid-liquid and solid-phase extraction. This extraction procedure involves the absorption of analytes into a polymeric film coated onto a fine silica fiber directly dipped in the aqueous sample. An SPME procedure for the determination of 12 organophosphorus pesticides in clean environmental water samples at low ng/ml concentration level has been developed by optimising variables involved in extraction and desorption. The absorption equilibrium has been estimated by mathematical treatment of the process using an expression that describes experimental absorption time profiles. The method was evaluated according to the reproducibility, linearity range and limits of detection using two different fiber coatings: 100 microm polydimethylsiloxane and 85 microm polyacrylate. The limits of detection obtained using nitrogen-phosphorus detection ranged between 0.01 and 0.2 ng/ml with relative standard deviations lower than 15% at the 1 ng/ml level. The method showed good linearity between 0.1 and 10 ng/ml with regression coefficients ranging between 0.97 and 0.999. Determination of organophosphorus pesticides in water samples in concentration below 0.1 ng/ml can be easily carried out with this fast, economic and solvent-free SPME procedure.

Adsorption↗

PubMed2004

Solid-phase microextraction of phenol compounds using a fused-silica fiber coated with beta-cyclodextrin-bonded silica particles.

A novel solid-phase microextraction (SPME) fiber was prepared by coating an HPLC beta-cyclodextrin bonded silica stationary phase (CDS) on the surface of a fused-silica fiber. The fiber was evaluated for the determination of five phenol compounds (phenol, 2,4-dimethylphenol, 4-nitrophenol, 3-chlorophenol, 4-methylphenol). Compared with commercially available polymer coatings, the CDS coating showed high sensitivity and fast velocity of mass transfer for phenol compounds because of its porous structure and a unique molecular structure of beta-cyclodextrin. In addition, the CDS coating was proved to be very stable at a relatively high temperature (up to 300 degrees C). The method was suitable for the determination of phenol compounds in aqueous samples. The determination of 4-nitrophenol in soil by microwave-assisted extraction (MAE) coupled to solid-phase microextraction was also investigated.

Journal Article↗

PubMed1995

Solid-phase microextraction for the determination of the free concentration of valproic acid in human plasma by capillary gas chromatography.

The potential of solid-phase microextraction in the bioanalysis of drugs is demonstrated. The free concentration of valproic acid in human plasma was determined by equilibrium dialysis at room temperature. To the dialysate was added an internal standard and the pH was adjusted to 2.5. The polymethylsiloxane-coated fused-silica fibre of the solid-phase microextraction device was inserted into the dialysate for 3 min. The sorbed analytes were then thermally desorbed at 210 degrees C in the split-splitless injection port of the gas chromatograph, separated on a Nukol capillary column and detected with a flame ionization detector. The method was shown to be highly reproducible with a detection limit of 1 microgram/ml of free valproic acid in human plasma.

Chromatography↗

PubMed2006

Determination of pyrethroid residues in tobacco by means of solid phase microextraction and GC/MS with the aid of ultrasonic assisted extraction using water as extracting solvent.

A rapid and simple sampling approach using solid phase microextraction (SPME) for pyrethroid residues analysis in flue-cured tobacco was studied. The fibers coated with poly-dimethylsiloxane (PDMS) at 100 microm thickness were chosen. Extraction time of 180 s, desorption time of 120 s and desorption temperature of 280 degrees C were selected. The whole sampling process, only including an ultrasonic assisted extraction step and a solid phase microextraction step, can be completed within 15 min. The associated SPME and ultrasonic assisted extraction using water as extracting solvent shows good results for tobacco pyrethroid residues determination. Results indicated that four pyrethroids can be determined simultaneously, and the limits of detection are below 35 ng g(-1) using GC/MS in selected ion monitoring (SIM) mode. The reproducibility of the technique is found to be better than 11.8% RSD.

Animals↗

PubMed2006

Determination of volatile oak compounds in aged wines by multiple headspace solid-phase microextraction and gas chromatography-mass spectrometry (MHS-SPME-GC-MS).

Multiple headspace solid-phase microextraction (MHS-SPME) with gas chromatography-mass spectrometry is proposed for quantification of nine volatile oak compounds in aged wines. These compounds are formed and extracted by wine when it is matured in oak barrels and are responsible for particular organoleptic properties and the high quality of these wines. Some important variables of the extraction process, for example volume of sample and extraction time, were studied. Extraction of 50 microL wine was performed with a divinylbenzene-Carboxen-polydimethylsiloxane fibre at 55 degrees C for 60 min. For calibration the same conditions were used, except that the wine was substituted by 50 microL of a standard solution in synthetic wine. The linearity, detection limits, and repeatability of the method were determined by use of standard solutions in synthetic wine. Detection limits were between 0.01 and 10 microg L(-1) (for eugenol and furfural, respectively) and repeatability, expressed as relative standard deviation, was from 2 to 6%. The method was used to analyse six red wines and the concentrations obtained were statistically compared with those obtained by the standard addition method for the same wines.

Gas Chromatography-Mass Spectrometry↗

PubMed2004

High pH-resistant, surface-bonded sol-gel titania hybrid organic-inorganic coating for effective on-line hyphenation of capillary microextraction (in-tube solid-phase microextraction) with high-performance liquid chromatography.

Sol-gel titania-poly(dimethylsiloxane) (TiO2-PDMS) coating was developed for capillary microextraction (CME) to perform on-line preconcentration and HPLC analysis of trace impurities in aqueous samples. A method is presented describing in situ preparation of the titania-based sol-gel PDMS coating and its immobilization on the inner surface of a fused silica microextraction capillary. To perform CME-HPLC, the sol-gel TiO2-PDMS capillary was installed in the HPLC injection port as an external sampling loop, and a conventional ODS column was used for the liquid chromatographic separation. The target analytes were extracted on-line by passing the aqueous sample through this sampling loop. The sol-gel titania-PDMS coated capillaries were used for on-line extraction and HPLC analysis of polycyclic aromatic hydrocarbons, ketones, and alkylbenzenes. The extracted analytes were then transferred to the HPLC column using an organic-rich mobile phase followed by HPLC separation via gradient elution. To our knowledge, this is the first report on the use of sol-gel titania-based organic-inorganic material as a sorbent in capillary microextraction. The newly developed sol-gel titania-based CME coatings demonstrated excellent pH stability and enhanced extraction capability over the commercial GC coatings that are conventionally used for the same purpose. Extraction characteristics of a sol-gel titania-PDMS capillary remained practically unchanged after continuous rinsing with a 0.1 M NaOH solution (pH 13) for 12h.

Chromatography, High Pressure Liquid↗

PubMed2002

Extending the solid-phase microextraction technique to high analyte concentrations: measurements and thermodynamic analysis.

The solid-phase microextraction (SPME) technique has been used historically to quantify analytes present at the parts per million level. However, the nonintrusive nature of SPME lends itself to other applications involving analytes at higher concentration. In the current work, the possibility of using the SPME technique to measure concentrated gaseous samples was examined. Pentane concentrations between 0 and 100% saturation were studied, over a temperature range of 20-45 degrees C. The results showed that, up to a critical mole fraction in the solid phase, the concentrations of pentane in the polymeric extracting solid and vapor phases were related by a constant, equal to Henry's constant. The temperature dependence of Henry's constant was shown to follow the predicted trend with temperature, as determined from rigorous thermodynamic calculations. Above the pentane concentration in the polymeric phase, the response deviated from linearity. The nonideality was captured in an activity coefficient. An activity coefficient model developed to describe the nonideality was found to be a function of the swollen volume of the SPME polymer phase. The results indicate that the SPME technique can be applied to high analyte concentrations, although difficulties may be encountered when multiple analytes are absorbed.

Journal Article↗

PubMed2004

Autonomous protein sample processing on-chip using solid-phase microextraction, capillary force pumping, and microdispensing.

A capillary force filling microsystem consisting of a chip-integrated solid-phase microextraction (SMEC) array and a microdispenser for sample purification and trace enrichment of peptides is described. The microextraction array was loaded with solid-phase media (50 microm Poros R2 beads) for purification and enrichment of proteomic samples. Samples bound to the SMEC were eluted in a volume of 200 nL. A piezo-electric microdispenser was docked to the array and the samples bound to the SMEC were eluted in a volume of 200 nL using capillary forces. The purified and enriched samples were dispensed onto the matrix-assisted laser desorption/ionization (MALDI) target, providing quality data from samples in the picomolar range. The nanoproteomic platform was compared to corresponding commercial preparation protocols, showing higher mass spectrometry (MS) signal intensities for peptides generated from an alpha-casein digest. The platform was also evaluated with regards to two-dimensional (2-D) gel-derived protein digests from both fibroblast and epithelial target cells.

Electrophoresis, Gel, Two-Dimensional↗

PubMed2006

Headspace solid-phase microextraction gas chromatography tandem mass spectrometry for the determination of brominated flame retardants in environmental solid samples.

A headspace solid-phase microextraction gas chromatography coupled with tandem mass spectrometry (HSSPME-GC-MS-MS) methodology for determination of brominated flame retardants in sediment and soil samples is presented. To the best of our knowledge, this is the first time that SPME has been applied to analyze polybrominated biphenyls (PBBs) and polybrominated diphenyl ethers (PBDEs) in environmental solid samples. Analyses were performed using 0.5-g solid samples moisturized with 2 mL water, employing a polydimethylsiloxane (PDMS) fiber coating, exposed to the headspace at 100 degrees C for 60 min. Several types of environmental solid samples were included in this study and the extraction efficiency was related to the organic matter content of the sample. Calibration was performed using real samples, and the method showed good linearity over a wide concentration range, precision, and afforded quantitative recoveries. The obtained detection limits were in the sub-ng g(-1) for all the target analytes in both samples. The proposed procedure was applied to several marine and river sediments and soils, some of which were found to contain PBDEs at concentrations in the ng g(-1) level; BDE-47, BDE-100, and BDE-99 were the major congeners detected. The proposed method constitutes a rapid and low-cost alternative for the analysis of the target brominated flame retardants in environmental solid samples, since the clean-up steps, fractionation, and preconcentration of extracts inherent to the classical multi-step solvent extraction procedures are avoided.

Journal Article↗

PubMed2004

Solid-phase microextraction and gas chromatography-mass spectrometry for the determination of polycyclic aromatic hydrocarbons in environmental solid matrices.

A solid-phase microextraction (SPME) and gas chromatography-mass spectrometry method for determining polycyclic aromatic hydrocarbons (PAHs) in environmental solid matrices is developed. Investigated matrices include seaweed (Undaria pinnatifida and Himanthalia elongata), humic substances (isolated from a wetland out-flow and purchased from Aldrich), and soil. Optimal conditions for a good SPME efficiency of 16 hydrocarbon compounds are obtained using a 100- micro m polydimethylsiloxane fiber directly immersed in aqueous carrier medium. The method is remarkable for presenting short extraction times and considerably high sensitivities. The SPME results obtained by using internal calibration give the total analyte concentration based on the identical partitioning behavior of native and spiked pollutants. The detection limits range from 0.001 to 0.1 mg of PAH per kilogram of dry matrix. SPME external calibration provides information regarding freely dissolved analytes. The detection limits range from 0.001 to 0.05 micro g of PAH per liter of carrier medium. The SPME with external calibration procedure can be applied to measure free concentrations of a target compound spiked into a carrier medium and onto a matrix. Based on a comparison of results obtained for the two samples, the partitioning of the target analyte between the matrix and the carrier medium is calculated.

Calibration↗

PubMed2005

Determination of methyl and ethyl esters of methanesulfonic, benzenesulfonic and p-toluenesulfonic acids in active pharmaceutical ingredients by solid-phase microextraction (SPME) coupled to GC/SIM-MS.

The development, optimization and validation of an extraction method for methyl and ethyl esters of various sulfonic acids is presented. The extraction and determination of these esters in active pharmaceutical ingredients (APIs) was accomplished using solid-phase microextraction coupled to GC/MS in the SIM mode. The factors affecting the extraction efficiency are discussed. This method was validated as a limits test and allows the determination of the sulfonic esters at the 5 ppm level in APIs. The method proved to be reproducible (%R.S.D.s less than 6%) and suitable for use with external standard quantitation, and also met basic validation requirements. This method offers numerous advantages over liquid-liquid extraction methods and was also compared to other extraction techniques such as solid-phase extraction (SPE) and liquid-phase microextraction (LPME) also being developed in our laboratories.

Benzenesulfonates↗

PubMed2004

Solid-phase microextraction gas chromatography-mass spectrometry determination of monoterpenes in honey.

Solid-phase microextraction (SPME) using a 100 microm poly(dimethylsiloxane) (PDMS) fiber, followed by gas chromatography (GC-MS) determination, has been applied to the analysis of some monoterpenoids in honey. The extraction was performed by direct immersion of the fiber using a sampling period of 15 min with constant magnetic stirring (1100 rpm) and an extraction temperature of 20 degrees C. A 7 mL sample volume of an aqueous solution of honey with 25% of NaCl was placed in 15 mL glass vial fitted with screw cap and PTFE/silicone septum. Desorption was performed directly in the gas chromatograph injector port during 5 min at 250 degrees C using the splitless mode. The method is sensitive with detection limits between 11 and 25 microg L(-1), precise with coefficients of variation in the range 1.28 and 3.71%, and linear over more than one order of magnitude. The related conditions were used for honey sample analyses with recoveries between 71.8 and 90.9%. SPME remains an attractive alternative technique due to its rapidity and because it is a solvent free extraction method.

Gas Chromatography-Mass Spectrometry↗

PubMed2001

A comparison of headspace entrainment on Tenax with solid phase microextraction for the analysis of the aroma volatiles of cooked beef.

Headspace solid phase microextraction (SPME), using a Carboxen-polydimethylsiloxane fiber, was compared with headspace entrainment on Tenax TA, as a means of examining the aroma constituents of cooked beef. Extracts were analyzed using gas chromatography-mass spectrometry. Headspace entrainment on Tenax extracted higher amounts of most volatiles, particularly low-boiling compounds. However, polar volatiles, such as hydroxyfuranones and hydroxyketones, were present at higher levels in the SPME extracts. Some components were present only in the SPME extracts, including norfuraneol, furaneol, and cyclotene, which are key Maillard reaction intermediates.

Animals↗

PubMed2004

Determination of pyrimethanil and kresoxim-methyl in soils by headspace solid-phase microextraction and gas chromatography-mass spectrometry.

A method using headspace solid-phase microextraction (HS-SPME) then gas chromatography-mass spectrometry with selected ion monitoring (GC-MS, SIM) has been developed for determination of trace amounts of the fungicides pyrimethanil and kresoxim-methyl in soil and humic materials. Both fungicides were extracted on to a fused-silica fibre coated with 85 microm polyacrylate (PA). Response-surface methodology was used to optimise the experimental conditions. For soil samples the linear dynamic range of application was 0.004-1.000 microg g(-1) for pyrimethanil and 0.013-1.000 microg g(-1) for kresoxim-methyl. The detection limits were 0.001 microg g(-1) and 0.004 microg g(-1) for pyrimethanil and kresoxim-methyl, respectively. HP-SPME-GC-MS analysis was highly reproducible-relative standard deviations (RSD) were between 6.7 and 12.2%. The method was validated by analysis of spiked matrix samples and used to investigate the presence of pyrimethanil and kresoxim-methyl above the detection limits in soil and humic materials.

Gas Chromatography-Mass Spectrometry↗