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At least 19 recordsLinked to original sources
PubMed1997

[Design and application of vacuum manifold for solid phase extraction].

Solid phase extraction (SPE) is now a common method for sample pretreatment. SPE vacuum manifold is a key instrument when SPE is used for sample pretreatment. It was developed by National Chromatographic R. & A. Center. Being connected with a vacuum pump, it can deal with 12 samples simultaneously. The manifold has a unique rotatable cover and can be conveniently rotated when switching between any two steps of SPE. An application of this SPE vacuum manifold in measuring bile acids in human serum was given.

Bile Acids and Salts↗
PubMed2002

In-line pressurized-fluid extraction-solid-phase extraction for determining phenolic compounds in grapes.

A new method of pressurized-fluid extraction coupled in-line with solid-phase extraction has been used for the extraction of phenolic compounds from grapes. The full extraction method is performed under an inert atmosphere. Five different solvents have been assayed using different extraction pressures and temperatures. Using two extraction stages with two different solvents, water and methanol, quantitative recovery for most of the assayed compounds has been found in the second extract. Only the most polar phenolic compound, gallic acid, was found distributed in both extracts. The application to real samples allows for a clean-up of the extracts. Cinnamic esters like caftaric acid, cis and trans-coutaric acids were found only in the methanolic extract. The reproducibility for the new method was measured using both an inert solid spiked with standards and grapes. Using between 202 and 424 microg of spiked standards, the resulting relative standard deviations were less than 5%, with the exception of gallic acid (RSD=13%). For grapes, the resulting RSD were 11% for trans-coutaric acid, 10% for caftaric acid and 6% for cis-coutaric acid.

Phenols↗
PubMed2006

Determination of benzoxazinone derivatives in plants by combining pressurized liquid extraction-solid-phase extraction followed by liquid chromatography-electrospray mass spectrometry.

A new analytical method based on the use of pressurized liquid extraction (PLE) followed by solid-phase extraction with LiChrolut RP C18 cartridges was evaluated for the sample preparation, extraction, and cleanup of eight naturally occurring benzoxazinone derivatives, 2-beta-D-glucopyranosyloxy-4-hydroxy-1,4-benzoxazin-3-one, 2-beta-D-glucopyranosyloxy-4-hydroxy-7-methoxy-1,4-benzoxazin-3-one, 2,4-dihydroxy-1,4-benzoxazin-3-one (DIBOA), 2,4-dihydroxy-7-methoxy-1,4-benzoxazin-3-one, 2-hydroxy-1,4-benzoxazin-3-one, 2-hydroxy-7-methoxy-1,4-benzoxazin-3-one, benzoxazolin-2-one, and 6-methoxybenzoxazolin-2-one in plant samples. Afterward, liquid chromatography-electrospray mass spectrometry, using the selected ion monitoring mode and internal standard (2-MeO-DIBOA, indoxyl-beta-D-glucoside, and quercetin-3-O-rutinoside) quantification method was performed. This paper demonstrates the effectiveness of the PLE method, in conjunction with sensitive and specific mass spectrometric detection, for the quantitative recovery of compounds of the benzoxazinone class from plants. The recoveries of the analytes ranged from 66 to 110% with coefficients of variation ranging from 1 to 14%. This method gave detection limits between 1 and 27 microg/g. The method was applied to foliage and roots of three different wheat cultivars, and the analytes were detected in the range of 11-3261 microg/g of dry weight.

Benzoxazines↗
PubMed2002

Automated sample preparation by pressurized liquid extraction-solid-phase extraction for the liquid chromatographic-mass spectrometric investigation of polyphenols in the brewing process.

The analysis of polyphenols from solid plant or food samples usually requires laborious sample preparation. The liquid extraction of these compounds from the sample is compromised by apolar matrix interferences, an excess of which has to be eliminated prior to subsequent purification and separation. Applying pressurized liquid extraction to the extraction of polyphenols from hops, the use of different solvents sequentially can partly overcome these problems. Initial extraction with pentane eliminates hydrophobic compounds like hop resins and oils and enables the straightforward automated on-line solid-phase extraction as part of an optimized LC-MS analysis.

Automation↗
PubMed2006

Establishing the feasibility of coupled solid-phase extraction-solid-phase derivatization for acidic herbicides.

The significance of this research is that it improves analytical methodology used for organic chemicals in aqueous solutions by establishing the feasibility of heterogeneous chemical derivatization at the liquid-solid interface (i.e., solid-phase reaction or solid-phase derivatization). A solid-phase derivatization method for determining chlorinated herbicide acids was developed. Solid-phase extraction was used to concentrate and retain analytes on sorbents for subsequent solid-phase derivatization. Background interferences were removed from the chromatograms by electronically subtracting the responses of blank, nonfortified analyses from spiked samples. Two extraction sorbents (octadecyl bonded silica and polystyrene-divinylbenzene) and two derivatizing reagents (BF3-MeOH and trimethylsilyldiazomethane) were investigated. Recovery of 13 chlorinated herbicide acids--including pentachlorophenol, dinoseb, and bentazon (having a derivatizable functional group, -OH or -NH, bonded directly to a phenyl group); dicamba, picloram, acifluorfen, 3,5-dichlorobenzoic acid, and dacthal (having a derivatizable functional group, -COOH, bonded directly to a phenyl group); and 2,4-D, 2,4,5-T, dichlorprop, 2,4,5-TP, and 2,4-DB (having a derivatizable functional group, -COOH, bonded directly to a sp3 carbon atom)--was tested. The analytical method developed was proven successful for determining acidic herbicides, except for the dacthal diacid metabolite, in aqueous samples.

Acids↗
PubMed2006

Analysis of anatoxin-a in biological samples using liquid chromatography with fluorescence detection after solid phase extraction and solid phase microextraction.

Anatoxin-a is a naturally occurring, potent neurotoxin produced by some species of cyanobacteria in freshwaters. This toxin, which is a potential health hazard, especially to animals, has been determined in different biological matrices such as several cyanobacterial cultures and water samples and carps and mussels tissue using a sensitive High Performance Liquid Chromatography with Fluorescence detection method. Sonication was the technique selected for the extraction of intracellular anatoxin-a and solid phase extraction using weak cation exchange was used for the concentration and purification of the samples. 4-Fluoro-7-nitro-2,1,3-benzoxadiazole (NBD-F) was used to convert anatoxin into a highly fluorescent derivative. Recovery experiments were performed for each type of matrix used in this work, and adequate values were obtained (71-87%). Limits of detection for anatoxin-a were estimated to be in the ng/L and ng/g level for water and cyanobacterial samples, respectively. The results obtained were also compared with those obtained after using solid phase microextraction, as an alternative for the extraction and purification of the samples. Advantages and disadvantages regarding to the efficiency for impurities removal, simplicity and rapidity and the potential for concentration enhancement of using both methodologies have been also discussed.

Chromatography, High Pressure Liquid↗
PubMed2006

Molecularly imprinted polymers for solid-phase extraction and solid-phase microextraction: recent developments and future trends.

Molecularly imprinted polymers (MIPs) are synthetic polymers having a predetermined selectivity for a given analyte, or group of structurally related compounds, that make them ideal materials to be used in separation processes. In this sense, during past years a huge amount of papers have been published dealing with the use of MIPs as sorbents in solid-phase extraction, namely molecularly imprinted solid-phase extraction (MISPE). Although the majority of these papers were restricted to describe the use of different templates for different applications, several attempts proposing new alternatives to minimize the inherent drawbacks of the preparation and use of MIPs (i.e. template bleeding, tedious synthesis procedure, etc.) have been reported. Thus, this paper does not pretend to be a collection of MISPE-related papers but to give an overview on the significant attempts carried out during recent years to improve the performance of MIPs in solid-phase extraction. In addition, the use of MIPs packed in high performance liquid chromatography (HPLC) columns for the direct injection of crude sample extracts and the preparation of imprinted fibres for solid-phase microextraction will be also discussed.

Combinatorial Chemistry Techniques↗
PubMed1995

Solid state NMR and extraction studies on "phenyl"-bonded stationary phases used for solid phase extraction.

The solid phase extraction (SPE) and elution of [14C]-propranolol from aqueous buffer has been studied for a range of phenyl-bonded SPE materials. Differences were noted in the recovery of the analyte using methanol-water eluents depending upon the manufacturer and whether or not phase had been endcapped. Efficient recoveries of [14C]-propranolol were only achieved when triethylamine was added to the eluting solvent as a competing base. Solid state cross polarisation/magic angle spinning (CP/MAS) NMR spectroscopy was used to characterise the phases further, which revealed differences in endcapping between materials as well as differences in the type and extent of cross-linking.

Magnetic Resonance Spectroscopy↗
PubMed2001

Fuel spill identification using solid-phase extraction and solid-phase microextraction. 1. Aviation turbine fuels.

The water-soluble fraction of aviation jet fuels is examined using solid-phase extraction and solid-phase microextraction. Gas chromatographic profiles of solid-phase extracts and solid-phase microextracts of the water-soluble fraction of kerosene- and nonkerosene-based jet fuels reveal that each jet fuel possesses a unique profile. Pattern recognition analysis reveals fingerprint patterns within the data characteristic of fuel type. By using a novel genetic algorithm (GA) that emulates human pattern recognition through machine learning, it is possible to identify features characteristic of the chromatographic profile of each fuel class. The pattern recognition GA identifies a set of features that optimize the separation of the fuel classes in a plot of the two largest principal components of the data. Because principal components maximize variance, the bulk of the information encoded by the selected features is primarily about the differences between the fuel classes.

Journal Article↗
PubMedDate not supplied

Comparison of solid-phase extraction and micro-solid-phase extraction for liquid chromatography/mass spectrometry analysis of pesticides in water samples.

Our recent on-line solid-phase extraction (SPE) device for micro-liquid chromatography, known as micro-solid-phase extraction (microSPE), was compared with traditional SPE for the analysis, from aqueous samples, of 4 pesticides belonging to different classes. Two different kinds of adsorbents, C18 and graphitized carbon black, were tested. A 2-stage ion trap mass spectrometer, equipped with homemade microflow electrospray ion (ESI) source, was used. Detection limits with a signal-to-noise ratio of 3:1 for both extraction methods were in the range of 0.1 microg/L for all compounds. However, better recoveries were obtained when microSPE traps were used.

Adsorption↗
PubMed2000

Kinetics of solid-phase extraction and solid-phase microextraction in thin adsorbent layer with saturation sorption isotherm.

The effects of sorbent saturation in thin adsorbent layers have been much overlooked in earlier research and should be taken into account in both the theory and practice of solid-phase extraction (SPE) and solid-phase microextraction (SPME). The adsorption kinetics of a single analyte into a thin adsorptive layer was modeled for several cases of agitation conditions in the analyzed volume. The extraction process in the adsorbent layer was modeled using a Langmuir isotherm approximated by the linear isotherm at low concentrations and by a saturation plateau at concentrations exceeding the critical saturation concentration. Laplace transformations were used to estimate the equilibration time and adsorbed analyte concentration profile for no agitation, practical and perfect agitation in the analyzed volume. The equilibration time may be significantly reduced at high degrees of oversaturation and/or agitation in the analyzed volume. The resulting models indicated that the adsorbent layer becomes saturated at some critical value of the oversaturation degree parameter. The critical value of the oversaturation parameter is affected by both the concentration of the analyte in the analyzed volume and the sorbent characteristics. It was also shown that the adsorption process is carried out via the propagation of the saturation adsorption boundary toward the inner boundary of the adsorbent layer. These new adsorption models should serve as "stepping stones" for the development of competitive adsorption kinetic models for both SPE and SPME, particularly in cases where fast sampling is used.

Chromatography, Liquid↗
PubMed2004

Solid-phase extraction versus solid-phase microextraction for the determination of chlorinated paraffins in water using gas chromatography-negative chemical ionisation mass spectrometry.

Solid-phase extraction (SPE) and solid-phase microextraction (SPME) were evaluated for the analysis of short-chain chlorinated paraffins (SCCPs) in water samples using gas chromatography coupled to negative chemical ionisation mass spectrometry (GC-NCI-MS). For SPE optimisation, four commercially available SPE cartridges were tested and several SPE parameters, such as the elution solvent, elution volume and breakthrough volume were studied. The best results were obtained with Varian Bond Elut-C18. In order to achieve a high selectivity in the determination of SCCPs, GC-NCI-MS was used. Quality parameters of the optimised SPE and SPME procedures were determined, and the best results were obtained for the SPE/GC-NCI-MS method with LODs of 5 and 20 ng l(-1) for tap and river water, respectively. This method was successfully applied to the analysis of SCCPs in river water samples at concentrations below the microg l(-1) level.

Chlorine↗
PubMed2004

Development of solid-phase extraction and solid-phase microextraction methods for the determination of chlorophenols in cork macerate and wine samples.

Tri-, tetra- and pentachlorophenol (TCP, TeCP and PCP) can be considered the precursors in the formation of corresponding chloroanisoles, known to be powerful odorants in corks and wine. Determining the presence of these chlorophenolic compounds in cork soaking solutions (ethanol/water mixtures, 12% (v/v) ethanol used for cork quality control testing), or in wine can be achieved by acetylation/gas chromatography electron-capture detection. In order to reach the required sensitivity, a previous preconcentration step is necessary. Solid-phase extraction (SPE) and headspace solid-phase microextraction (HS-SPME) have given good results for the preconcentration of TCP, TeCP and PCP in such matrices. The use of Oasis HLB cartridges gives acceptable recoveries for the three compounds when different volumes (50-250 mL) of cork macerate with concentrations ranging from 20 to 150 ng/L are processed. Preconcentration based on HS-SPME has also been optimised with a 100 microm polydimethylsiloxane fibre and in situ derivatization. The HS-SPME method allows chlorophenols in a cork soaking solution and in wine to be determined with a limit of detection of 1 ng/L for each compound (in cork macerate) and a repeatability of around 0.5%-5% (n=8) for a concentration level of 30 ng/L.

Chlorophenols↗
PubMed2004

Comparison of extraction of a beta-blocker from plasma onto a molecularly imprinted polymer with liquid-liquid extraction and solid phase extraction methods.

An optimised solid phase extraction (SPE) method developed for the extraction of a structural analogue of the beta-blocking drug propranolol from plasma utilising a molecularly imprinted polymer (MIP) has been compared with methods based on conventional liquid-liquid extraction (LLE), and SPE using C18-bonded and immobilised phenyl boronic acid (PBA). All four methods could be used for the extraction of the analyte with acceptable accuracy and precision. The MIP-based method, unlike the other methods required a protein precipitation step prior to extraction to eliminate the effects of co-extracted protein. The best performance was seen with the LLE method followed by SPE on the C18 phase. The MIP-based method represented no advantage over the comparator methods for this analyte. Indeed the performance of the MIP-based method was marginally worse as leaching of low level template impurities prevented detection of the target analyte at low concentrations (5 ngmL(-1)). This relatively poorer performance was evident as worse accuracy at low concentrations with a consequent higher limit of quantification than the conventional methods.

Adrenergic beta-Antagonists↗
PubMed2005

Cost analysis of ELISA, solid-phase extraction, and solid-phase microextraction for the monitoring of pesticides in water.

The implementation of a pesticide water monitoring program in South Africa is limited by a lack of financial and analytical resources. A cost analysis of three analytical methods, enzyme-linked immunosorbent assays (ELISA), solid-phase microextraction (SPME), and traditional solid-phase extraction methods (SPE), was conducted. The cost analysis assumed a hypothetical scenario in terms of the sampling area (a grape farming rural region in the Western Cape province of South Africa), sample collection (weekly grab samples collected from eight sites by an environmental health officer in a nearby town), transport of samples (via courier), and analysis (endosulfan and chlorpyrifos analysis conducted by a local higher educational institution laboratory in Cape Town). The cost per sample for the three analytical methods was determined by estimating the annual capital costs, including building and equipment, and recurrent costs, including transport, personnel, supplies, and building operating costs. At the optimal utility of resources, SPME had the lowest cost per sample (US $37), followed by SPE (US $48.50) and ELISA (US $60). Recurrent costs formed the bulk of the costs of all three methods (91-97%). The cost of supplies was particularly high for ELISA (US $34 per sample). The cost per sample estimated for all three methods is substantially lower than those quoted by other laboratories in South Africa. The low cost of SPME is particularly important because of the sensitivity and reliability of this method and the faster output compared to SPE, and SPME is recommended for the long-term monitoring of pesticide pollution.

Chlorpyrifos↗
PubMed2002

Comparison of solid-phase extraction and solid-phase microextraction for carbofuran in water analyzed by high-performance liquid chromatography-photodiode-array detection.

In this study a direct solid-phase microextraction (SPME) procedure has been developed for the determination of carbofuran in water. Experimental parameters such as selection of SPME coating, effect of temperature, effect of salt addition and solvent desorption were studied and optimized. Analytical parameters such as linearity, precision, detection and quantitation limits, and matrix effects for solid-phase extraction (SPE) and SPME methods were evaluated for comparison purposes with the aim of selecting the most appropriate depending on the detection capabilities required. SPE and SPME were followed by high-performance liquid chromatography with diode-array detection, using a 50 x 4.6 mm I.D. guard column and a 150 x 4.6 mm I.D. analytical column, both packed with C18 silica. Both methods can be applied to real samples and give the same results, but SPE allows the detection of lower carbofuran concentrations (0.06 microg/L) as compared to

Carbofuran↗
PubMed2006

Ethanol/Water extraction combined with solid-phase extraction and solid-phase microextraction concentration for the determination of chlorophenols in cork stoppers.

The appearance of 2,4,6-trichloroanisole (TCA) in cork stoppers is of great concern because it can cause off-flavors in bottled wine. To prevent this sensorial defect, there should not be any traces of 2,4,6-trichlorophenol (TCP), 2,3,4,6-tetrachlorophenol (TeCP), or pentachlorophenol (PCP) in the finished corks, because they are the direct precursors of TCA. In the course of this study two methodologies based upon an extraction with ethanol/water mixtures to determine the chlorophenolic content in cork matrices were developed. The cork extract is preconcentrated using both solid-phase extraction and solid-phase microextraction methodologies. The latter was optimized by applying a full two-level factorial design. Finally, spiked ground corks at nanogram per gram levels of each chlorophenol were analyzed under optimal conditions and by applying both procedures. The obtained results demonstrate that chlorophenols can be detected in corks contaminated at the nanogram per gram level and, thus, these approaches can be successfully applied as quality control measures in the cork industry.

Chlorophenols↗
PubMed1993

Determination of mizolastine, a new antihistaminic drug, in human plasma by liquid-liquid extraction, solid-phase extraction and column-switching techniques in combination with high-performance liquid chromatography.

For the determination of mizolastine (2-[[[1-[(4-fluorophenyl)methyl]-1H-benzimidazol-2-yl]-4- piperidinyl]methylamino]-4(3H)-pyrimidinone, SL 85.0324), a new antihistaminic drug, in human plasma, three methods were developed based on liquid-liquid extraction, solid-phase extraction and column-switching in combination with high-performance liquid chromatography with ultraviolet detection. The liquid-liquid extraction method included a back-extraction step that preconcentrates the drug into a small aqueous volume, resulting in very high sensitivity (0.5 ng/ml of plasma); it can be used in conventional bioanalytical laboratories that do not have sophisticated automatic devices. The solid-phase extraction method is performed by using a robotic system (Benchmate). It is completely automated from the initial sampling to the final injection into the chromatograph. It has a good sensitivity (1 ng/ml of plasma), but requires an expensive apparatus and skilled analysts. The column-switching method is based on a solid-phase extraction performed on-line with chromatographic analysis; it is not completely automatic, because some operations are performed manually. The device required for valve switching is not expensive and can be managed by a simple integrator or a personal computer; it is very easy to use and affords a sensitivity (2.5 ng/ml of plasma) that generally satisfies the needs of pharmacokinetic investigations of mizolastine. The conditions were similar for all the three methods: a C8 type column, an eluent of phosphate buffer and acetonitrile, and a spectrophotometric ultraviolet detector operated at 285 nm.

Autoanalysis↗