SEARCH · Search PubMed

Results for “Liquid Phase Microextraction”

Search indexed PubMed citations on genomics, clinical trials, systematic reviews and public health. Explore titles, authors and supplied subject terms, then open the PubMed record.

SourceResearch connectionFrom yearThrough year

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 235 records · Page 13Linked to original sources

PubMed2006

Fast gas chromatography of explosive compounds using a pulsed-discharge electron capture detector.

The detection of a mixture of nine explosive compounds, including nitrate esters, nitroaromatics, and a nitramine in less than 140 sec is described. The new method employs a commercially available pulsed-discharge electron capture detector (PDECD) coupled with a microbore capillary gas chromatography (GC) column in a standard GC oven to achieve on-column detection limits between 5 and 72 fg for the nine explosives studied. The PDECD has the benefit that it uses a pulsed plasma to generate the standing electron current instead of a radioactive source. The fast separation time limits on-column degradation of the thermally labile compounds and decreases the peak widths, which results in larger peak intensities and a concomitant improvement in detection limits. The combination of short analysis time and low detection limits make this method a potential candidate for screening large numbers of samples that have been prepared using techniques such as liquid-liquid extraction or solid-phase microextraction.

Journal Article↗

PubMed2001

Biotransformation of (R)-(+)- and (S)-(-)-limonene by fungi and the use of solid phase microextraction for screening.

The biotransformation of (R)-(-)- and (S)-(-)-limonene by fungi was investigated. More than 60 fungal cultures were screened for their ability to bioconvert the substrate, using solid phase microextraction as the monitoring technique. After screening, the best fungal strains were selected for further study and were grown as sporulated surface cultures in conical flasks and as submerged liquid cultures. It was found that (+)- and (-)-limonene were converted by Penicillium digitatum to alpha-terpineol (main metabolite), cis- and trans-p-menth-2-en-1-ol, neodihydrocarveol and limonene oxide (minor metabolites) using liquid cultures. The bioconversion of (R)-(-)- and (S)-(-)-limonene by Corwespora cassiicola yielded (1S,2S,4R)- and (1R,2R,4S)-limonene-1,2-diol respectively. The bioconversions by liquid cultures were also monitored by solid phase microextraction as a function of time. The optimum conversion of limonene to alpha-terpineol by Penicillium digitatum was obtained after 8 hours (yield up to 100%). Since an important pH-decrease was noticed in some liquid broths, the stability of limonene under acidic conditions was investigated. No acid catalysed conversion products were recovered after 8 days from control flasks at pH 3.5 containing limonene.

Ascomycota↗

PubMed2000

Separation methods for amino group-possessing pesticides in biological samples.

The separation methods for pesticides include liquid-liquid extraction, solid-phase extraction and solid-phase microextraction, gas chromatography (GC), GC-mass spectrometry (MS), GC-MS-MS, high-performance liquid chromatography (LC), LC-MS and LC-MS-MS. This review deals with each technique commonly used for extraction, chromatographic separation and detection of amino group possessing pesticides, such as diazines, triazines, carbamates, dinitroanilines and chloroacetanilides in biological samples. The methods presented for analysis of the pesticides in complicated biological matrices seem to be easily applicable to surface or groundwater in environmental chemistry.

Chromatography, Gas↗

PubMed2003

Evaluation of Kd underestimation using solid phase microextraction.

Many important environmental pollutants are strongly adsorbing hydrophobic compounds. Because of their potential to adsorb to dissolved organic matter (DOM), their partition coefficient Kd may be underestimated by the conventional approach due to incomplete phase separation. In this study, solid-phase microextraction (SPME) was compared with liquid-liquid partition (LLP) for measuring Kd of bifenthrin and permethrin isomers on sediments. Due to its selective detection of the freely dissolved concentration, SPME gave Kd values 0.6-4.4-fold greater than those obtained by LLP in creek and field sediments and 3.6-21.7-fold greater in nursery runoff sediments. Underestimation by the conventional method was attributed to adsorption to DOM that was not excluded from the aqueous phase by centrifugation. The degree of underestimation was dependent on the source and amount of DOM and may be generally significant for compounds that have DOM adsorption coefficient (KDOM) > 10(4). This study provides evidence that the existing Kd values for many hydrophobic pollutants may be underestimated, and SPME may be a viable, efficacious tool for evaluating the underestimation.

Adsorption↗

PubMed2004

The effects of sample preparation and gas chromatograph injection techniques on the accuracy of measuring guaiacol, 4-methylguaiacol and other volatile oak compounds in oak extracts by stable isotope dilution analyses.

The deuterium-labeled standards [(2)H(3)]-guaiacol and [(2)H(3)]-4-methylguaiacol were synthesized and utilized in a method employing gas chromatography-mass spectrometry to determine the concentration of guaiacol and 4-methylguaiacol in wine or extracts of oak shavings. The method was combined with previously published methods for 4-ethylphenol, 4-ethylguaiacol, cis- and trans-oak lactone and vanillin, so that all these compounds could be quantified in a single analysis. The method can employ either liquid-liquid extraction or headspace solid-phase microextraction (SPME) and is rapid, robust, precise, and accurate. Under certain conditions, there was artifactual generation, to varying degrees, of guaiacol, 4-methylguaiacol, cis-oak lactone, and vanillin during the analysis of oak extracts, especially when diethyl ether extraction and injector block temperatures at or above 225 degrees C were employed. The most substantial effects were observed for guaiacol, in which results could be exaggerated by over 10 times. These artifacts could be avoided by using headspace SPME or by preparing liquid-liquid extracts with pentane or pentane/diethyl ether (2:1) injected at 200 degrees C providing spot checks using headspace SPME were performed. Data obtained for previously published quantitative determination of guaiacol in oak extracts should be reexamined carefully, with special attention paid to their respective methods of sample preparation and analysis.

Chromatography, Gas↗

PubMed2004

Two-step liquid-liquid-liquid microextraction of nonsteroidal antiinflammatory drugs in wastewater.

A simple and novel two-step liquid-liquid-liquid microextraction technique combined with reversed-phase HPLC has been developed for the determination of the nonsteroidal antiinflammatory drugs ibuprofen and 2-(4-chlorophenoxy)-2-methylpropionic acid in wastewater samples. In the first step, the analytes were extracted from an acidified sample (donor solution) into 1-octanol immobilized in the pores of 10 pieces of polypropylene hollow fiber and further into a basic acceptor phase inside the hollow fiber channels. This first extraction step, using 0.01 M NaOH as the acceptor phase and 0.1 M HCl within the donor phase, had a 100% relative recovery with an enrichment factor of 100-fold. The extract in the first step was then adjusted to acidic condition with HCl. It now represented the donor phase for the second step of the extraction, using a single piece of hollow fiber, with 2 microL of 0.01 M NaOH solution as the acceptor phase. This analyte-enriched acceptor phase was subsequently withdrawn into a microsyringe and directly injected into an HPLC system for analysis. With this two-step microextraction, sensitivity enhancement of >15,000-fold could be obtained. Detection limits of < or =100 ng/L could be achieved for both compounds. The method was applied to the analysis of wastewater.

Anti-Inflammatory Agents, Non-Steroidal↗

PubMed2001

Changes in the aroma of a strawberry drink during storage.

The flavor of a commercially available strawberry drink was investigated with special regard to the changes of the sensory properties during the shelf life of the product. The experiments were performed using gas chromatographic methods after liquid-liquid extraction and after solid-phase microextraction of the headspace. A trained sensory test panel was used to substantiate the results from instrumental analyses. The relative concentrations of several compounds were followed over a storage period of six weeks at elevated temperature (37 degrees C), which corresponds to about 12 months storage at room temperature. Significant concentration changes of several flavor compounds were determined after a short storage time. These results correlate highly with changes in the aroma observed by the sensory test panel. Further on, changes in the sensorial relevance of aroma active compounds were monitored by comparative aroma extract dilution analysis of extracts of the fresh product and the product at the end of the declared shelf-life time. The results showed a significant decrease in flavor dilution factors of compounds with characteristic fruity attributes.

Beverages↗

PubMed2006

Sample extraction method combining micellar extraction-SPME and HPLC for the determination of organochlorine pesticides in agricultural soils.

A method for the determination of organochlorine pesticides in soil samples combining microwave assisted micellar extraction (MAME) with solid-phase microextraction (SPME) and high-performance liquid chromatography-UV has been developed. A mixture of two nonionic surfactants (polyoxyethylene 10 lauryl ether and polyoxyethylene 10 stearyl ether) was used for the extraction of pesticides from agricultural soils, and different types of SPME fibers were compared. The different parameters which affect extraction efficiency in the SPME procedure were optimized such as extraction time and temperature. The method developed involves extraction and preconcentration for the target analytes in soil samples. The analytical parameters were also studied and good recoveries obtained, RSD being lower than 10% and detection limits ranging between 36 and 164 ng g(-1) for the pesticides studied. The proposed method was successfully applied to the determination of some organochlorine pesticides in several kinds of agricultural soil samples with different characteristics.

Agriculture↗

PubMed2006

Biomarker discovery by imaging mass spectrometry: transthyretin is a biomarker for gentamicin-induced nephrotoxicity in rat.

Adverse drug effects are often associated with pathological changes in tissue. An accurate depiction of the undesired affected area, possibly supported by mechanistic data, is important to classify the effects with regard to relevance for human patients. MALDI imaging MS represents a new analytical tool to directly provide the spatial distribution and the relative abundance of proteins in tissue. Here we evaluate this technique to investigate potential toxicity biomarkers in kidneys of rats that were administered gentamicin, a well known nephrotoxicant. Differential analysis of the mass spectrum profiles revealed a spectral feature at 12,959 Da that strongly correlates with histopathology alterations of the kidney. We unambiguously identified this spectral feature as transthyretin (Ser(28)-Gln(146)) using an innovative combination of tissue microextraction and fractionation by reverse-phase liquid chromatography followed by a top-down tandem mass spectrometric approach. Our findings clearly demonstrate the emerging role of imaging MS in the discovery of toxicity biomarkers and in obtaining mechanistic insights concerning toxicity mechanisms.

Amino Acid Sequence↗

PubMed2003

Systematic error in automated in-tube solid-phase microextraction.

The widely employed configuration for automated in-tube solid-phase microextraction (SPME) involves modification of a commercial liquid chromatographic autosampler into an automated extraction device. This popular configuration is demonstrated to result in an inherent systematic error in the quantitation of analyte in a given matrix. The source of error is traced to the accumulation of analyte in the extraction and the pre-extraction segment (i.e., sample loop, metering valve and tubing prior to the metering valve) of the autosampler where the analyte comes in contact with the residual mobile phase. This results in cross-contamination due to sample/mobile phase mixing. The quantity of analyte accumulated in these segments is shown to consistently increase with the increasing number of draw/eject cycles. As a result of the accumulation, the amount of analyte recorded leads to inaccurate quantitative information, leading to overestimation of the limit of detection and limit of quantitation, when automated in-tube SPME is employed as an approach for sample enrichment. Insertion of a 100-microl air plug prior to extraction step was able to significantly minimize sample/mobile phase mixing of analyte with the residual mobile phase in the pre-extraction and extraction step, thus minimizing the systematic error.

Automation↗

PubMed2003

Determination of triazines in soil by microwave-assisted extraction followed by solid-phase microextraction and gas chromatography-mass spectrometry.

A method for determining triazine herbicides in soil samples that combines microwave-assisted extraction with solid-phase microextraction is described. Water containing 1% methanol was employed as extractant. The parameters of solid-phase microextraction and microwave-assisted extraction were investigated. In solid-phase microextraction, particular attention was paid to the negative effect of salt on fiber stability. Our experiments showed that this effect could be effectively reduced by simply washing the fiber with deionized water. The selected triazines could be efficiently extracted by the aqueous extractant at 105 degrees C for 3 min, with 80% output of maximum power (1,200 W). The extraction procedure provided good precision (<7%) and recoveries (76.1-87.2%). The limits of detection were in the range 2-4 microg/kg. Compared with conventional liquid extraction, microwave-assisted extraction-solid-phase microextraction was more efficient, accurate and faster, and used a very small amount of organic solvent (only 250 microL methanol). The extraction of aged spiked soil samples indicated that, although the recoveries were lower than those of freshly spiked samples, they were nevertheless satisfactory for the quantitative analysis of real-world samples.

Gas Chromatography-Mass Spectrometry↗

PubMed2000

Analysis of low-volatility organic sulphur compounds in wines by solid-phase microextraction and gas chromatography.

A method for analysing low-volatility sulphur compounds using solid-phase microextraction has been developed. The analytes were extracted directly from the liquid sample using fibres coated with different stationary phases. The best extraction efficiency was obtained with Carboxen-polydimethylsiloxane coating. Ionic strength, sample volume, time and temperature of the extraction were optimised and the matrix effect studied. The method enables 15 sulphur compounds in wine to be determined at trace levels with recoveries close to 100% and limits of detection between 0.05 and 5 microg/L. The overall method was successfully applied to the determination of the sulphur compounds studied in several red, white and rosé wines.

Chromatography, Gas↗

PubMed2000

[From medicolegal toxicology to forensic toxicology].

The importance of forensic toxicology has been increasing until now, because of the increasing numbers of toxic substances and poisoning incidents. In Japan, a special translational word "houi-chudoku-gaku" has been used for the forensic toxicology especially in the field of legal medicine. The Japanese word, however, does not seem appropriate for translation of forensic toxicology, because it covers medicine, pharmacy and police sciences interdisciplinary. In 1980, Emeritus Prof. Hidetoshi Yoshimura created an appropriate word "hochudoku-gaku" for translation of forensic toxicology. In 1982, Prof. Yoshimura and his friends established the Japanese Association of Forensic Toxicology, consisting of people from legal medicine, pharmacy and police institutes. This Association enabled lively discussions among different fields and greatly contributed to advances of forensic toxicology in Japan. We started studies of forensic toxicology using gas chromatography (GC)/mass spectrometry (MS) in 1979. Until now, we delt with solid-phase extraction (1987-1994), surface ionization GC (1989-1997), negative ion chemical ionization MS (1981-now), solid-phase microextraction (1994-now), cryogenic oven trapping GC (1997-now), surface ionization organic MS (1998-now) and high-performance liquid chromatography/tandem MS (1998-now). In this review, the author presents some details of solid-phase microextraction, negative ion chemical ionization MS, cryogenic oven trapping GC and surface ionization organic MS. Unprecedented poisoning terrorism by use of sarin took place in Matsumoto and Tokyo in 1994 and 1995, respectively. On July 25, 1998, a curry poisoning incident using arsenious acid occurred in Wakayama, resulting in the death of 4 people and injury of 63 people. Since then, more than 30 imitative poisoning cases have been reported by mass communication within 1 year. In spite of the above continuing poisoning cases, almost no effective measures have been taken by the administration of our country and local governments. Many serious problems concerning poisoning and drug abuse are accumulating in Japan. In this review, the problems are also made manifest, and some proposals are presented to solve the problems.

Forensic Medicine↗

PubMed1997

Rapid determination of corticosteroids in urine by combined solid phase microextraction/liquid chromatography/mass spectrometry.

Solid-phase microextraction combined with fast short-column liquid chromatography/mass spectrometry (SPME/LC/MS) was used for isolating and analysing 11 corticosteroids and 2 steroid conjugates from urine samples. Several SPME parameters such as polarity of fibres, extraction time and effect of ionic strength, were investigated, and their impact on the SPME/LC/MS technique was studied. To demonstrate the potential of the SPME/LC/MS method, its application to the determination of steroids in human urine was investigated. The method was shown to be sensitive with detection limits between 4 and 30 ng/mL and precision between 4.9 and 11.1% RSD through the use of an internal standard technique. The versatility of the method was also exhibited by its excellent linearity in the concentration range of 20 to 20,000 ng/mL in urine for all investigated compounds. A comparison of the SPME/LC/MS method with LC/MS methods utilizing traditional sample preparation techniques, shows that the former offers similar performance in terms of precision, linearity and detection limits, but is clearly easier to use and faster to perform.

Adrenal Cortex Hormones↗

PubMed1998

Rapid SPME/LC/MS/MS analysis of N-methylcarbamate pesticides in water.

Solid-phase microextraction combined with fast short-column liquid chromatography/electrospray ionization tandem mass spectrometry (SPME/LC/MS/MS) was used for isolating and analyzing nine N-methylcarbamate pesticides from water samples. Several SPME parameters, such as polarity of fibers, extraction time, and effect of ionic strength, were investigated and their impact on the SPME/LC/MS/MS technique was studied. The method was shown to be sensitive with detection limits between 0.3 and 1.9 microg/L and reproducible with precision between 4.5 and 12.7% RSD. The versatility of the method was exhibited by its excellent linearity in the concentration range of 2-2,000 microg/L in drinking water. A comparison of the SPME/LC/MS/MS method with LC/MS/MS methods utilizing traditional sample preparation techniques shows that the former offers similar performance in terms of precision and linearity, but is clearly easier to use and faster to perform.

Adsorption↗

PubMed1999

Use of solid-phase microextraction for the analysis of bisphenol A and bisphenol A diglycidyl ether in food simulants.

A new method has been developed to simultaneously analyse bisphenol A (BPA) and bisphenol A diglycidyl ether (BADGE) in aqueous based food simulants. The method consists on direct immersion solid-phase microextraction (SPME) of the analytes from the liquid matrix and subsequent chromatographic analysis by gas chromatography-mass spectrometry. Using the proposed method, a whole analysis (including chromatographic step) can be completed in less than 40 min, with minimum sample handling. The SPME method shows good analytical performance for simultaneous BPA and BADGE analysis, except for BADGE determination in the aqueous alcohol (simulant C) solution. Detection limits ranging from 0.1 to 2.0 ng/g for BPA and from 13 to 15 ng/g from BADGE were obtained, with a linear range from the low-ng/g to several-microg/g range for BPA and from 0.1 microg/g to 40 microg/g for BADGE. A possible optimisation method has been also developed and introduced.

Benzhydryl Compounds↗

PubMed2002

A new procedure for solid-phase microextraction using a flow-through system with air segmentation.

Three different procedures for solid-phase microextraction (SPME) of trace organic compounds from liquids were evaluated: simple extraction with magnetic stirring, use of a laboratory-made flow-through extraction cell and a new system based on a laboratory-made flow-through extraction cell in which the sample stream is segmented with air bubbles. In this new procedure, the sample flows through the cell as a regular sequence of small plugs separated by air bubbles instead of in a continuous stream. This new system combines the advantages of SPME, as a simple, fast, sensitive and solvent-free sample concentration/introduction technique, with the advantages of on-line processing of aqueous sample as a less time-consuming, efficient and continuous technique. For testing the new flow-through procedure, a mixture of phthalate esters was used for direct absorption from an aqueous solution with a 100 microm polydimethylsiloxane fiber. The efficiency and precision of the procedure were compared with those of extraction with magnetic stirring and the usual flow-through cell concept. The results indicate better contact of the analytes with the extraction film when the air-segmented flow-through extraction cell is employed.

Journal Article↗

PubMed2001

Sample treatment in chromatography-based speciation of organometallic pollutants.

Speciation analysis is nowadays performed routinely in many laboratories to control the quality of the environment, food and health. Chemical speciation analyses generally include the study of different oxidation state of elements or individual organometallic compounds. The determination of the different chemical forms of elements is still an analytical challenge, since they are often unstable and concentrations in different matrices of interest are in the microg l(-1) or even in the ng l(-1) range (e.g., estuarine waters) or ng g(-1) in sediments and biological tissues. For this reason, sensitive and selective analytical atomic techniques are being used as available detectors for speciation, generally coupled with chromatography for the time-resolved introduction of analytes into the atomic spectrometer. The complexity of these instrumental couplings has a straightforward consequence on the duration of the analysis, but sample preparation to separate and transfer the chemical species present in the sample into a solution to be accepted readily by a chromatographic column is the more critical step of total analysis, and demands considerable operator skills and time cost. Traditionally, liquid-liquid extraction has been employed for sample treatment with serious disadvantages, such as consumption, disposal and long-term exposure to organic solvent. In addition, they are usually cumbersome and time-consuming. Therefore, the introduction of new reagents such as sodium tetraethylborate for the simultaneous derivatization of several elements has been proposed. Other possibilities are based in the implementation of techniques for efficient and accelerated isolation of species from the sample matrix. This is the case for microwave-assisted extraction, solid-phase extraction and microextraction, supercritical fluid extraction or pressurized liquid extraction, which offer new possibilities in species treatment, and the advantages of a drastic reduction of the extraction time and the embodiment into on-line flow analysis systems. This new generation of treatment techniques constitutes a good choice as fast extraction methods for feasible species-selective analysis of organometallic compounds under the picogram level, that can be used for national regulatory agencies, governmental and industrial quality control laboratories, and consequently, for manufacturers of analytical instrumentation.

Chromatography↗