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J A Jönsson

Publications and source records attributed to J A Jönsson.

At least 19 recordsLinked to original sources

Analysis of PAH compounds in soil with on-line coupled pressurised hot water extraction-microporous membrane liquid-liquid extraction-gas chromatography.

Pressurised hot water extraction (PHWE) was coupled on-line with microporous membrane liquid-liquid extraction (MMLLE) and gas chromatography (GC) in the analysis of polycyclic aromatic hydrocarbon (PAH) compounds in soil. The MMLLE serves as a trapping device after the PHWE. Water from PHWE is directed to the donor side of the membrane unit and the analytes are extracted to the acceptor solution on the other side of the membrane. The role of MMLLE is to clean and concentrate the extract, which is then transferred on-line to the GC via a sample loop and an on-column interface using partially concurrent solvent evaporation. Separate optimisation of MMLLE and simulations of the PHWE-MMLLE connection were carried out before the actual on-line coupling. After optimisation of the whole on-line system, the efficiencies of the PHWE-MMLLE-GC and PHWE-solid-phase trap extractions were compared. The PHWE-MMLLE-GC method allowed on-line analysis of soil samples. The method was linear, with limits of detection in the range 0.05-0.13 ng and limits of quantification 0.65-1.66 microg g(-1). Comparison of the results with those obtained by other techniques confirmed the good performance.

Chemical Fractionation↗

Routine analysis of alcohol and nonylphenol polyethoxylates in wastewater and sludge using liquid chromatography-electrospray mass spectrometry.

A wide range of alcohol and nonylphenol polyethoxylates was determined by separation on a reversed-phase liquid chromatographic column, followed by electrospray ionisation-mass spectral analysis. The compounds were separated chromatographically according to their aliphatic chain length. The mass spectral analysis functioned as a second separation step during which homologues of the ethoxylates were separated according to their polyethoxylate chain length. In this manner a truly orthogonal separation was obtained. The compounds were detected as ammonium complexes. The analysis presented is capable of qualitative and quantitative determination of a large number of ethoxylates as well as their metabolites in a single run. The method was applied to many different sample types, ranging from primary and treated wastewater to sludge. Batches of 50 real samples were routinely analysed without the need for cleaning the mass spectrometer or regeneration of the column. By utilising the extracted mass chromatograms, detection limits of 1 to 10 microg/l could be obtained for individual compounds in water samples, while the detection limits were around 100 microg/kg in sludge, depending on the degree of pollution.

Alcohols↗

Supported liquid membrane extraction of peptides.

The application of supported liquid membrane (SLM) extraction for the enrichment of short peptides is presented. The extraction efficiency is dependent on the pH of donor phase and salt concentration in acceptor phase. Moreover, the extraction efficiency is also influenced by the peptide amino-acid sequence and hydrophobicity.

Biochemistry↗

Membrane-based techniques for sample enrichment.

Sample preparation techniques based on non-porous membrane extraction generally offer a high degree of selectivity and enrichment power, together with convenient possibilities for direct and automated connections to chromatographic and other analytical instruments. In this review principles and applications for techniques as supported liquid membrane extraction, microporous membrane liquid-liquid extraction, polymeric membrane extraction and membrane extraction with a sorbent interface are described and compared.

Body Fluids↗

Determination of thiophanate-methyl and its metabolites at trace level in spiked natural water using the supported liquid membrane extraction and the microporous membrane liquid-liquid extraction techniques combined on-line with high-performance liquid chromatography.

On-line supported liquid membrane (SLM) extraction and microporous membrane liquid-liquid extraction (MMLLE) techniques for sample preparation of natural water samples have been developed for the determination of thiophanate-methyl (TM), carbendazim (MBC) and 2-aminobenzimidazole (2-AB) using reversed-phase HPLC. The combination of SLM extraction and MMLLE offers extraction conditions that makes it possible to determine a wide variety of compounds, i.e., permanently charged, ionisable and non-polar at sub ppb level. The detection limits obtained after extraction are about 0.1 microg/l for MBC and 2-AB using SLM, and 0.5 x Lg/l for TM using MMLLE and the precision is better than 5% for both systems. Typical enrichment rates are 0.6 and 2.7 times/min using SLM and MMLLE, respectively.

Chromatography, High Pressure Liquid↗

Automated liquid membrane extraction for high-performance liquid chromatography of Ropivacaine metabolites in urine.

An automatic method for the determination of metabolites of Ropivacaine in urine was set up. It utilizes supported liquid membrane extraction for sample clean-up and enrichment, followed by ion-pair chromatography determination using UV detection. The extraction was very selective with no observed interfering compounds from the urine matrix, permitting simple isocratic chromatographic analysis. The detection limits for spiked urine samples were 2-18 nM for the different compounds. The repeatability was 1-3% (RSD) with an internal standard that was also extracted, and about twice without this standard. A throughput of 3.3 samples per hour was achieved and the liquid membrane was stable for more than a week.

Amides↗

Microporous membrane liquid-liquid extraction coupled on-line with normal-phase liquid chromatography for the determination of cationic surfactants in river and waste water.

Membrane-based continuous liquid-liquid extraction combined on-line with normal-phase liquid chromatography is proposed for the determination of cationic surfactants in complex aqueous samples. The technique has the potential for complete automation. Selective enrichment of cationic surfactants from spiked river water and waste-water samples with simultaneous removal of matrix constituents, followed by a quantitative transfer of the extract onto a liquid chromatographic column and separation of the surfactant homologues yielding low detection limits, has been realised. The homologues of alkyldimethylbenzylammonium chloride (Dodigen 226) were chosen as model compounds in the method development. Dodigen homologues were ion-paired with heptanoic acid and extracted into chlorobutane by means of microporous membrane liquid-liquid extraction. It was thereby possible to attain an enrichment of over 250 times for one of the homologues, viz. the concentration in the organic liquid is 250 times higher than in the original sample. Detection limits for the three best-detected homologues of the mixture were in the range 0.7-5 microg/l in spiked river water samples. Ion-pair normal-phase liquid chromatography, again with heptanoic acid as counter-ion, gave the necessary separation of the surfactant homologues.

Cations↗

Alpha1-microglobulin chromophores are located to three lysine residues semiburied in the lipocalin pocket and associated with a novel lipophilic compound.

Alpha1-microglobulin (alpha1m) is an electrophoretically heterogeneous plasma protein. It belongs to the lipocalin superfamily, a group of proteins with a three-dimensional (3D) structure that forms an internal hydrophobic ligand-binding pocket. Alpha1m carries a covalently linked unidentified chromophore that gives the protein a characteristic brown color and extremely heterogeneous optical properties. Twenty-one different colored tryptic peptides corresponding to residues 88-94, 118-121, and 122-134 of human alpha1m were purified. In these peptides, the side chains of Lys92, Lys118, and Lys130 carried size heterogeneous, covalently attached, unidentified chromophores with molecular masses between 122 and 282 atomic mass units (amu). In addition, a previously unknown uncolored lipophilic 282 amu compound was found strongly, but noncovalently associated with the colored peptides. Uncolored tryptic peptides containing the same Lys residues were also purified. These peptides did not carry any additional mass (i.e., chromophore) suggesting that only a fraction of the Lys92, Lys118, and Lys130 are modified. The results can explain the size, charge, and optical heterogeneity of alpha1m. A 3D model of alpha1m, based on the structure of rat epididymal retinoic acid-binding protein (ERABP), suggests that Lys92, Lys118, and Lys130 are semiburied near the entrance of the lipocalin pocket. This was supported by the fluorescence spectra of alpha1m under native and denatured conditions, which indicated that the chromophores are buried, or semiburied, in the interior of the protein. In human plasma, approximately 50% of alpha1m is complex bound to IgA. Only the free alpha1m carried colored groups, whereas alpha1m linked to IgA was uncolored.

Animals↗

On-line microporous membrane liquid-liquid extraction for sample pretreatment combined with capillary gas chromatography applied to local anaesthetics in blood plasma.

A new automated procedure for analyzing complex samples has been developed utilizing microporous membrane liquid-liquid extraction (MMLLE) combined with capillary gas chromatography. Some local anaesthetics were used as model compounds in aqueous solution as well as in blood plasma. The MMLLE procedure was performed in a flow system with the sample fed to the donor side of the hydrophobic microporous membrane and with an organic solvent (hexane) in the pores and as the acceptor solution. The analytes in a small volume of sample (< 1 mL) were extracted into the organic acceptor phase which was transferred into the gas chromatographic system by utilizing a loop-type interface compatible with large-volume (300 microL) injection. High selectivity and low carry-over effects were obtained with the system. The detection limits were 0.5-1 ng/mL using 0.5 mL of human plasma, and the precision was approximately 5%. The effects of pH, flow rates, and adsorption of the analytes were evaluated.

Adsorption↗

On-line supported liquid membrane-liquid chromatography with a phenol oxidase-based biosensor as a selective detection unit for the determination of phenols in blood plasma.

The potential of on-line combination of supported liquid membrane extraction and column liquid chromatography with a phenol oxidase-based biosensor as a selective detection unit has been investigated for the determination of phenols in human plasma. The phenols are selectively extracted into a porous PTFE (polytetraflouroethene) membrane impregnated with a water-immiscible organic solvent and further into an alkaline acceptor phase. Via an ion-exchange interface, the analytes are transferred to a reversed-phase column where they are separated and detected using the biosensor. No sample pretreatment before the extraction, except centrifugation, is made. Due to the high selectivity both in the extraction and in the detection steps and to the fact that the demands on the chromatographic separation are low, a quick separation using an eluent with a low concentration of organic modifier can be made, without affecting the biosensor response. Detection limits below the 50 microg/l level in blood plasma were obtained for the three model compounds, phenol, p-cresol and 4-chlorophenol.

Biosensing Techniques↗

Miniaturized supported liquid membrane device for selective on-line enrichment of basic drugs in plasma combined with capillary zone electrophoresis.

A hollow fiber miniaturized supported liquid membrane (SLM) device for sample preparation is connected on-line with capillary electrophoresis and used for determination of a basic drug, bambuterol, in human plasma. The analyte is extracted from the outside of the hollow fiber (donor) through the liquid membrane (pores of the fiber impregnated with organic solvent) into the acceptor solution in the fiber lumen. The process is driven by differences in pH between the donor and acceptor solution. The whole volume of the acceptor solution can then be injected into the CZE capillary by using the double-stacking procedure for large volume-injection. Very clean extracts of low ionic strength are obtained from the SLM treatment, making this sample pretreatment method compatible with the CZE double-stacking procedure, which in turn makes it possible to inject large volumes of sample onto the separation capillary. Good performance of the whole procedure is demonstrated, and detection limits in the low nanomolar range were obtained in spite of the relatively weak UV absorbance of bambuterol. Extractions through the miniaturized SLM unit can be performed for 5-6 h without regenerating the fiber. The regeneration procedure was tested, and no relevant changes in the performance of the extraction could be found after seven regenerations, allowing the same fiber to be used for a week.

Electrophoresis, Capillary↗

Determination of a basic drug, bambuterol, in human plasma by capillary electrophoresis using double stacking for large volume injection and supported liquid membranes for sample pretreatment.

In this work we show the potential of using a double stacking procedure based on field enhancement as a means to increase the concentration sensitivity in CZE analysis of human plasma extracted by the supported liquid membrane (SLM) technique. A basic drug, bambuterol, was used as a model substance. The low ionic strength of the SLM extract makes this pretreatment technique compatible with the double stacking sequence. No significant loss of separation performance was observed when 3 microliters of SLM extract was concentrated by the CZE double stacking sequence. Almost no visible difference was seen between the electropherograms after enrichment of a plasma blank and an aqueous blank. Good performance of the whole procedure was demonstrated and detection limits in the low nM range were obtained in spite of the relatively weak UV absorbance of bambuterol. The developed procedure was evaluated for both achiral and chiral separation. In the latter approach chiral selectivity was obtained by adding cyclodextrin to the separation electrolyte.

Bronchodilator Agents↗

Liquid membrane work-up of blood plasma samples applied to gas chromatographic determination of aliphatic amines.

A technique for sample work-up and enrichment using a supported liquid membrane in an automated flow system, connected to a gas chromatograph, was used for the determination of aliphatic amines in human blood plasma. The amines studied were N,N-dimethylethylamine, triethylamine, N-methylmorpholine, cyclohexylamine and N,N-dimethylcyclohexylamine. An efficient clean-up of the complex plasma matrix was achieved, resulting in identical blank chromatograms for plasma samples and aqueous solutions. Different parameters influencing the efficiency and selectivity of the extraction procedure were experimentally studied and theoretically explained. The detection limit depends on the extraction flow-rate and the available sample volume. With 1 ml of sample and a flow-rate giving an extraction time of 16 min, the detection limit was ca. 5 ppb (5 micrograms/l); with 4 ml of sample and a lower flow-rate, sub-ppb detection limits could be reached in ca. 3 h. Linear calibration curves up to 500 ppb were obtained. Blood plasma samples from volunteers exposed to N,N-dimethylethylamine in air were analysed, and the results compared favourably with independent measurements by another method.

Amines↗

Asthma as a child. Symptom-free as an adult?

Of 123 individuals hospitalized as children (aged 5-15 years) because of asthma over a 10-year period (1953-1962), four are dead of whom three died of asthma at follow-up 23-31 years later. Using a survey questionnaire, 64 (53%) of the 117 responders (response rate 98%) claimed to be completely symptom-free. The rest were still suffering from their disease. Of the 31 symptom-free individuals still living in the community, two had decreased lung volumes and seven had positive methacholine provocation tests at re-examination, thus indicating hyperreactivity. Twenty-five individuals showed both positive skin prick tests and Phadiatop allergy tests. Nineteen individuals were suffering from allergic rhinoconjunctivitis. So, of symptom-free adults hospitalized for asthma in childhood, nearly a quarter (23%) had hyperreactive airways. The occurrence of positive skin prick test/Phadiotop and rhinoconjunctivitis was, however, even higher (80% and 61% respectively), thereby indicating that the disappearance of allergy may not be a prerequisite for restoration to health in asthma.

Adolescent↗

Controlled thermal degradation for the identification and quantification of amine N-oxides in urine.

Studies of amine N-oxides in urine are important for the evaluation of occupational exposure to amines. These thermolabile compounds are difficult to handle by either gas or liquid chromatography, so a device for controlled thermal degradation has therefore been developed. It consists of a short precolumn with shut-off valves at both ends and an aluminum block for heating, and it was connected to the injection port of a gas chromatograph. After injection of amine N-oxides onto the precolumn and thermal degradation, the degradation products were allowed to enter the analytical column. Trimethylamine N-oxide (TMAO) and triethylamine N-oxide (TEAO) were investigated. Their thermal degradation patterns could be used for identification and quantification in aqueous solutions and in urine. Linear calibration graphs based on degradation product peaks (trimethylamine and O,N,N-trimethylhydroxylamine from TMAO and diethylamine and triethylamine from TEAO) were obtained for concentrations up to 500 ppm. Detection limits in aqueous solutions were 0.2 ppm (ca. 1 ng) for TMAO and 1 ppm for TEAO and the precisions were 6% and 9%, respectively. In urine, similar values were obtained for TEAO. The detection limit for TEAO corresponds to the expected concentration in urine after an 8-h exposure to air containing 0.8 mg/m3 of triethylamine.

Amines↗

The long-term prognosis of childhood asthma in a predominantly rural Swedish county.

In 1985 a survey questionnaire was sent to 119 individuals who had been hospitalized as children (aged 5-15) because of asthma over a ten-year period (1953-1962). Four patients out of 123 had died, three of them because of asthma. The response rate was 98% and the follow-up covered a time range from 23 to 31 years. The mean age at follow-up was 33 (range 26-43) and sixty-four individuals (55%) were free from symptoms. The severity of asthma was evaluated by means of a symptom-score divided into 5 degrees (no symptoms to continuous asthma). Symptom onset under the age of 4, the occurrence of atopic eczema and increased sensitivity to pollen, furry animals and respiratory tract infections correlated significantly (p less than 0.05, p less than 0.05 and p less than 0.01, respectively) with the occurrence of continuous adult asthma. A factor which appears to predict the development of adult asthma is a high level of medical care, expressed as the number of days of hospitalization during childhood.

Adult↗