PubMed Health⌕ Search

SEARCH · PubMed Health

Results for “Solid Phase Extraction”

Explore indexed PubMed citations for clinical trials, systematic reviews and public health research. Read source abstracts and follow each citation to its original PubMed record.

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

At least 37 records · Page 2Linked to original sources
PubMed2002

Optimization of solid-phase extraction and solid-phase microextraction for the determination of alpha- and beta-endosulfan in water 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 to measure residues of pesticides 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 required. Although solid-phase extraction (SPE) is the most common technique for isolation and concentration of pesticides from water, solid-phase microextraction (SPME) is being increasingly applied for this purpose. In this study, a direct-SPME procedure has been developed for the determination of alpha-endosulfan and beta-endosulfan in waters; experimental parameters such as selection of SPME coating, effect of temperature, effect of salt addition, optimization of the sample volume, adsorption and desorption profiles and desorption temperature were studied and optimized. Analytical parameters such as linearity, precision, detection and quantitation limits, and matrix effects for SPE and SPME methods were evaluated for comparison purposes with the aim of selecting the most appropriate for a certain application. Both extraction techniques, SPE and SPME, were followed by gas chromatography with electron-capture detector.

Chromatography, Gas↗
PubMed1997

[The enrichment of polycyclic aromatic hydrocarbons in water samples by solid-phase extraction].

Solid-phase extraction (SPE) is an emerging chromatographic sample preparation technique. The novel extraction technique can reduce the time and volume of organic solvents required, and alleviate problems associated with the formation of emulsions as compared to conventional liquid-liquid extractions. This study was designed to demonstrate the utility of SPE for trace enrichment of polycyclic aromatic hydrocarbons (PAHs) in water samples. The results showed that dichloromethane and benzene are the preferred elution solvents for the adsorbed PAHs. The recoveries of PAHs with SPE are in the range of 87% to 102%. When the elution solvent is selected, the variation of recoveries as a function of the volume of elution solvent used can be determined. Meanwhile, further studies showed that recoveries become worse as the number of rings of PAH increased. The decrease of solubility and adsorption onto container surface may be responsible for bad recoveries. The addition of 20% (V/V) methanol or ethanol into the sample prior to spiking can greatly improve the recoveries of larger PAHs. Recoveries of 89%-108% can be obtained.

Polycyclic Aromatic Hydrocarbons↗
PubMed2000

Ion-pair solid-phase extraction.

Solid-phase extraction (SPE) is a technique widely employed by analytical chemists. SPE cartridges are available in a wide variety of formats containing media with diverse chemistries. This paper will review ion-pair SPE, one of the less frequently applied, and presumably less well-known techniques. Advantages of this technique over more conventional reversed-phase or ion-exchange SPE include selectivity, compatibility with rapid evaporative concentration, and potential application to multiclass multiresidue analysis.

Chromatography, Ion Exchange↗
PubMed2001

Monofluorinated polycyclic aromatic hydrocarbons as internal standards to monitor trace enrichment and desorption of their parent compounds during solid-phase extraction.

Solid-phase extraction (SPE) is an established sample-preparation technique for clean-up procedures of polycyclic aromatic hydrocarbons (PAHs). The suitability of monofluorinated polycyclic aromatic hydrocarbons (F-PAHs) as a novel set of internal standards, was tested for two widely used SPE sorbents, octyl-bonded silica and styrene-divinylbenzene copolymer. The elution profiles of eight F-PAHs and their parent PAHs, taken from the priority pollutant list of the US-Environmental Protection Agency, were compared for demineralized water and waste water. In both instances, the match of the elution profiles was exceptionally close. The eight F-PAHs and the corresponding PAHs were determined by reversed-phase liquid chromatography using acetonitrile-water gradient elution with UV detection at 254 nm. The UV spectra of the F-PAHs show a small bathochromic shift compared with the parent PAHs.

Chromatography, Liquid↗
PubMed2005

Behaviour of carbamate pesticides in gas chromatography and their determination with solid-phase extraction and solid-phase microextraction as preconcentration steps.

This work reports a study of the chromatographic behaviour of seven carbamate pesticides (aldicarb, carbetamide, propoxur, carbofuran, carbaryl, methiocarb, and pirimicarb) by gas chromatography-mass spectrometry (GC-MS). Variables such as injector temperature, solvent, injection mode, and the degree of ageing of the chromatographic column were studied. One of the aims of this work was to achieve a controlled decomposition of carbamates by a solid-phase microextraction (SPME) preconcentration step with a polyacrylate fibre in order to obtain reproducible chromatographic signals of the degradation products. Optimisation of the SPME process was accomplished by means of experimental design. Several methods using ultrapure water were developed with different preconcentration configurations: SPME-GC-MS, SPE followed by SPME-GC-MS, and SPE plus GC-MS. For all the pesticides studied, method detection limit (MDL) values below 0.1 microg L-1 were reached in at least one of the proposed configurations.

Carbamates↗
PubMed2002

Online coupling of pressurized liquid extraction, solid-phase extraction and high-performance liquid chromatography for automated analysis of proanthocyanidins in malt.

A new instrumental setup for automated extraction of solid samples by online coupling of pressurized liquid extraction, automated SPE (solid-phase extraction) and HPLC is presented. From the extraction to the chromatogram no manual sample handling is required. The application to the determination of proanthocyanidins in malt reduces time and manual work to a minimum compared to former manual methods. Twenty samples can be processed within 24 h in respect to eight samples with the manual method. Using the features of the instrumental coupling, an optimized strategy for SPE of proanthocyanidins from natural samples was developed, requiring no evaporation step, using commercial cartridges and delivering concentrated eluates. The recovery of five main malt proanthocyanidins was 97%, with a reproducibility of 5%. This new instrumental coupling is thought to reduce time and costs along with improved results for a broad range of solid sample materials.

Anthocyanins↗
PubMed2004

Development of a sensitive methodology for the analysis of chlorobenzenes in air by combination of solid-phase extraction and headspace solid-phase microextraction.

In this study, a combination of solid-phase extraction (SPE) and solid-phase microextraction (SPME) has been used to determine chlorobenzenes in air. Analytes were sampled by pumping a known volume of air through a porous polymer (Tenax TA). Then, the adsorbent was transferred into a glass vial and SPME was performed. The quantification was carried out using gas chromatography (GC)-electron-capture detection or GC-MS. Several SPME coatings (100 microm poly(dimethylsiloxane) (PDMS), 75 microm Carboxen (CAR)-PDMS, 65 microm PDMS-divinylbenzene (DVB), 65 microm PDMS-DVB and 85 microm polyacrylate (PA) were evaluated, obtaining the highest responses with Carbowax (CW)- PDMS for the most volatile chlorobenzenes, and with PDMS-DVB or CW-DVB fibers for the semivolatile compounds. To optimize some other factors that could affect the SPME step, a factorial design was used. Kinetic studies of the SPME process were also performed. Concerning the SPE step, breakthrough was studied, showing that 2.5 m3 of air could be processed without losses of the most volatile compounds. The performance of the method was evaluated. External calibration, which does not require the complete sampling process, demonstrated to be suitable, obtaining good linearity (R2 > 0.99) for all chlorobenzenes. Recovery studies were performed at two concentration levels (4 and 40 ng/m3), obtaining quantitative recoveries (>80%). Limits of detection at the sub ng/m3 were achieved for all the target compounds.

Air↗
PubMed1999

Quantification of the xenoestrogens 4-tert.-octylphenol and bisphenol A in water and in fish tissue based on microwave assisted extraction, solid-phase extraction and liquid chromatography-mass spectrometry.

Extraction methods were developed for quantification of the xenoestrogens 4-tert.-octylphenol (tOP) and bisphenol A (BPA) in water and in liver and muscle tissue from the rainbow trout (Oncorhynchus mykiss). The extraction of tOP and BPA from tissue samples was carried out using microwave-assisted solvent extraction (MASE) followed by solid-phase extraction (SPE). Water samples were extracted using only SPE. For the quantification of tOP and BPA, liquid chromatography mass spectrometry (LC-MS) equipped with an atmospheric pressure chemical ionisation interface (APCI) was applied. The combined methods for tissue extraction allow the use of small sample amounts of liver or muscle (typically 1 g), low volumes of solvent (20 ml), and short extraction times (25 min). Limits of quantification of tOP in tissue samples were found to be approximately 10 ng/g in muscle and 50 ng/g in liver (both based on 1 g of fresh tissue). The corresponding values for BPA were approximately 50 ng/g in both muscle and liver tissue. In water, the limit of quantification for tOP and BPA was approximately 0.1 microg/l (based on 100 ml sample size).

Animals↗
PubMed2001

Determination of phenylurea herbicides in natural waters at concentrations below 1 ng l(-1) using solid-phase extraction, derivatization, and solid-phase microextraction-gas chromatography-mass spectrometry.

A procedure is presented which allows the ultratrace level determination of phenylurea herbicides (PUHs) in natural waters. Samples were enriched by solid-phase extraction (SPE) on Carbopack B and alkylated with iodoethane and sodium hydride to yield thermostable products. After derivatization, the aqueous samples were extracted and injected by SPME. The use of iodoethane instead of iodomethane allowed the differentiation between parent compounds and the N-demethylated metabolites. Limits of detection were between 0.3 and 1.0 ng/l for the parent compounds. Standard deviations below 10% were achieved for samples containing more than 4 ng/l in very different matrices including Nanopure water, lake water, and waste water treatment plant (WWTP) effluent. Moreover, the para-hydroxylated metabolite of diuron could be quantified with the same procedure. The presence of further metabolites was assessed qualitatively. Chromatography was stable over a large number of measurements even with dirty samples from WWTP effluent. The precision and sensitivity of the developed analytical method allowed the investigation of the fate of PUHs in lakes, their degradation during drinking water treatment and their transport within the North Sea.

Calibration↗
PubMed1996

High-performance liquid chromatography determination of pyrimethamine, dapsone, monoacetyldapsone, sulfadoxine, and N-acetyl-sulfadoxine after rapid solid-phase extraction.

A solid-phase extraction procedure and a corresponding high-performance liquid chromatographic technique based on methods previously published by Edstein et al. (Edstein M. Quantification of antimalarial drugs. I. Simultaneous measurement of sulphadoxine, N4acetylsulphadoxine and pyrimethamine in human plasma. J Chromatogr 1984;305:502-7; Edstein M. Quantification of antimalarial drugs. II. Simultaneous measurement of dapsone, monoacetyldapsone and pyrimethamine in human plasma. J Chromatogr 1984;307:426-31) were developed for simultaneous determination of either dapsone (DDS), monoacetyldapsone (MADDS), and pyrimethamine (PYR) or sulfadoxine (SDX), N-acetyl-sulfadoxine (NAS) and pyrimethamine in plasma. Solid-phase extraction was achieved using C-18 extraction columns. An ionpair chromatography was performed on a C-18 analytical column (mu Bondapak C-18, 300 x 3.9 mm I.D.). Gradient elution with methanol, acetonitrile, PIC B6 reagent (1-hexanesulphonic acid), and water as mobile phase was applied. Ultraviolet detection was done at 210 nm for PYR, at 254 nm for SDX and NAS, and at 295 nm for DDS and MADDS. The extraction recoveries averaged 92.1% for PYR, 87.6% for DDS, 87.5% for MADDS, 91.2% for SDX, and 92.4% for NAS. The limit of quantification using 1.0-ml plasma samples was 15 ng/ml for PYR, DDS, MADDS, NAS, and 25 ng/ml for SDX (precision < 15%).

Anti-Infective Agents↗
PubMed2000

Quantitative separation of aliphatic and aromatic hydrocarbons using silver ion--silica solid-phase extraction

A solid-phase extraction (SPE) method employing silver nitrate impregnated silica has been developed and evaluated for the separation of defined aliphatic and aromatic hydrocarbons from crude oils. The versatility of the SPE method is demonstrated using a light crude oil from the North Sea and a heavy crude oil from Orcutt field (Monterey, California, U.S.A.). The coefficients of variation for a number of geochemical parameters measured on both aliphatic and aromatic hydrocarbons were excellent. The separation efficiency of SPE is demonstrated using quantification of monoaromatic steroid hydrocarbons which are notoriously difficult to efficiently sequester into the aromatic hydrocarbon fraction using traditional liquid chromatographic procedure. The selectivity and efficiency of the SPE technique is comparable with that of silica gel TLC. However, losses of volatile compounds such as naphthalene are limited during SPE since the sample remains in solvent. We conclude that solid-phase extraction affords rapid sample turnover suitable for processing large sample numbers with high reproducibility.

Journal Article↗
PubMed2006

[Determination of trace haloacetic acids in drinking water using ion chromatography coupled with solid phase extraction].

The combined solid phase extraction (SPE)-ion chromatography (IC) method was developed for the analysis of trace haloacetic acids (HAAs) in drinking water. The tested HAAs included monochloroacetic acid (MCAA), dichloroacetic acid (DCAA), trichloroacetic acid (TCAA), monobromoacetic acid (MBAA) and dibromoacetic acid (DBAA). For trace determination of HAAs in real drinking water samples, conditions of LiChrolut EN SPE cartridge were investigated for HAAs preconcentration and matrix elimination. Elution was carried out by 2 mL of sodium hydroxide (10 mmol/L) with the flow rate of 2 mL/min. The Dionex IonPac AS16 column (250 mm x 4 mm i. d.), a high capacity and hydroxide-selective anion-exchange column designed for the determination of polarizable anions, was chosen for chromatographic separation. HAAs were analyzed with a concentration gradient of NaOH with the flow rate of 0.8 mL/min and detected by suppressed conductivity. A 500 microL sample loop was used. The detection limits of this SPE-IC method for MCAA, DCAA, DBAA and TCAA were 0.38-1.69 microg/L and MBAA was 12.5 microg/L under 25-fold preconcentration. The results demonstrate that the method is suitable for the analysis of trace haloacetic acids in drinking water.

Acetates↗
PubMed1992

Comparison of solvent extraction and solid-phase extraction for the determination of organochlorine pesticide residues in water.

Solid-phase extraction (SPE) of organochlorine pesticide residues from environmental water samples was evaluated using octadecyl (C18)-bonded porous silica. The efficiency of SPE of these pesticide residues from reagent water samples at 1-5 micrograms dm-3 levels was compared with those obtained by solvent extraction with hexane and Freon TF (trichlorotrifluoroethane). Average recoveries exceeding 80% for these organochlorine pesticides were obtained via the SPE method using small cartridges containing 100 mg of 40 microns C18-bonded porous silica. The average recovery by solvent extraction with hexane and Freon TF exceeded 90% in both instances. It was concluded that the recoveries and precision for the SPE of organochlorine pesticides were poorer than those for the solvent extraction method. Organochlorine pesticide residue levels in environmental water samples from two major rivers flowing through predominantly rice-growing areas were monitored by gas chromatography using the solvent extraction method with hexane. Exceptionally high levels of organochlorine pesticide residues such as BHC, DDT, heptachlor, endosulfan and dieldrin were found in these water samples.

Chromatography, Gas↗
PubMed2002

Effect of solvents on the selectivity of terbutylazine imprinted polymer sorbents used in solid-phase extraction.

A solid-phase extraction sample preparation method using a molecularly imprinted polymer (MIP) selective for the triazine type pesticide terbutylazine has been developed. The method involves preconcentration from large volumes of water samples on a C18 disk coupled to selective clean-up on the MIP. The method has been optimised by studying the recovery and retention of terbutylazine and some other structurally related triazine derivates as a function of the selective washing solvent used. The effect of the water content of the selective washing solvent was also investigated on the recovery of the MIP. River water samples were analysed with the coupled technique, and efficient clean-up of the samples was observed.

Polymers↗
PubMed2002

Determination of phenols in landfill leachate-contaminated groundwaters by solid-phase extraction.

A solid-phase extraction method for phenols in landfill leachates was developed and optimized in order to solve the expected and observed problems associated with an anaerobic matrix containing high concentrations of salts and organic matter. Isolute ENV+ cartridges exhibited the best retention of phenols of the four sorbents examined, and was the only cartridge which a 1 L leachate sample could pass through. With the other cartridges, clogging made this impossible. The final method, which included 27 different phenols, gave detection limits of <0.1 microg/L (drinking water concentration limit for pesticides) for most phenols (25), and for 12 phenols <0.01 microg/L. Recovery rates (determined for four concentrations in the range 1-25 microg/L, two replicates of each) were in the range 79-104% (SD 1-12%), except for phenol (26+/-1.3%) and 2-methoxyphenol (62+/-4.2%). Up to 12 different phenols could be identified in leachates from three Danish landfills, ranging in concentration from 0.01 to 29 microg/L, which is at the lower end of the concentration range usually found for phenols in landfill leachates (sub-microg/L to mg/L).

Phenols↗