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  • 1.
    Bossi, A
    et al.
    University Verona, Department Agriculture and Ind Biotechnol, I-37134 Verona, Italy; Cranfield University, Institute BioScience and Technology, Cranfield MK43 0AL, Beds, England; .
    Piletsky, SA
    University Verona, Department Agriculture and Ind Biotechnol, I-37134 Verona, Italy; Cranfield University, Institute BioScience and Technology, Cranfield MK43 0AL, Beds, England; .
    Righetti, PG
    University Verona, Department Agriculture and Ind Biotechnol, I-37134 Verona, Italy; Cranfield University, Institute BioScience and Technology, Cranfield MK43 0AL, Beds, England; .
    Turner, APF
    Cranfield University, UK.
    Capillary electrophoresis coupled to biosensor detection2000In: Journal of Chromatography A, ISSN 0021-9673, E-ISSN 1873-3778, Vol. 892, no 02-jan, p. 143-153Article in journal (Refereed)
    Abstract [en]

    The present review highlights some modern aspects of biosensor revelation, a detection method which has already found a large number of applications in healthcare, food industry and environmental analysis. First, the concept of bio-recognition, which is at the heart of biosensor technology, is discussed, with emphasis on host-guest-like recognition mechanisms. This detection device has been successfully coupled, in its first applications, to chromatographic columns, which allow a high resolution of complex mixtures of analytes prior to interaction with the biosensing unit. The properties of the transducing elements, which should generate a signal (e.g., electrochemical, thermal, acoustic, optical) of proper intensity and of relative fast rise, are additionally evaluated and discussed. The review then focuses on potential applications of biosensing units in capillary electrophoresis (CE) devices. CE appears to be an excellent separation methodology to be coupled to biosensor detection, since it is based on miniaturized electrophoretic chambers, fast analysis times, complete automation in sample handling and data treatment and requires extremely small sample volumes. Although only a few applications of CE-based biosensors have been described up to the present, it is anticipated that this hyphenated technique could have a considerable expansion in the coming years, (C) 2000 Elsevier Science B.V. All rights reserved.

  • 2.
    Bossi, Alessandra
    et al.
    Department of Science and Technology, University of Verona, Verona, Italy.
    Castelletti, Laura
    Department of Science and Technology, University of Verona, Verona, Italy.
    Piletsky, Sergey A.
    Institute of BioScience and Technology, Cranfield University at Silsoe, Silsoe, Bedfordshire, UK.
    Turner, Anthony P. F.
    Cranfield University, UK.
    Righetti, Pier Giorgio
    Department of Science and Technology, University of Verona, Verona, Italy.
    Properties of poly-aminophenylboronate coatings in capillary electrophoresis for the selective separation of diastereoisomers and glycoproteins2004In: Journal of Chromatography A, ISSN 0021-9673, E-ISSN 1873-3778, Vol. 1023, no 2, p. 297-303Article in journal (Refereed)
    Abstract [en]

    The polymerisation of 3-aminophenylboronic acid (APBA) in aqueous environment has been used for the open tubular modification of capillary electrophoresis (CE) capillaries. Being poly-APBA endowed with boronic acid, aromatic rings and secondary amines groups, it posses a variety of functional groups affecting selectivity. Diastereoisomers (e.g. ascorbic and isoascorbic acid) and proteins (e.g. haemoglobins) were successfully separated onto poly-APBA column, by means of a combination of electrophoresis and open tubular electrochromatography. The mechanism of selection was investigated: results indicate an interplay between enhancing or silencing the contribution of the protonable functionahties (amino groups, boronic acid). The properties of APBA polymer coating make it attractive for CE separation and for further application in affinity separations and chip technologies.

  • 3.
    Concheiro, Marta
    et al.
    NIDA, MD 21224 USA.
    Castaneto, Marisol
    NIDA, MD 21224 USA; University of Maryland Baltimore County, MD 21228 USA.
    Kronstrand, Robert
    Linköping University, Department of Medical and Health Sciences, Division of Radiological Sciences. Linköping University, Faculty of Medicine and Health Sciences. National Board Forens Med, Department Forens Genet and Forens Toxicol, Linkoping, Sweden.
    Huestis, Marilyn A.
    NIDA, MD 21224 USA.
    Simultaneous determination of 40 novel psychoactive stimulants in urine by liquid chromatography-high resolution mass spectrometry and library matching2015In: Journal of Chromatography A, ISSN 0021-9673, E-ISSN 1873-3778, Vol. 1397, p. 32-42Article in journal (Refereed)
    Abstract [en]

    The emergence of novel psychoactive substances is an ongoing challenge for analytical toxicologists. Different analogs are continuously introduced in the market to circumvent legislation and to enhance their pharmacological activity. Although detection of drugs in blood indicates recent exposure and link intoxication to the causative agent, urine is still the most preferred testing matrix in clinical and forensic settings. We developed a method for the simultaneous quantification of 8 piperazines, 4 designer amphetamines and 28 synthetic cathinones and 4 metabolites, in urine by liquid chromatography coupled to high-resolution mass spectrometry (LC-HRMS). Data were acquired in full scan and data dependent MS2 mode. Compounds were quantified by precursor ion exact mass, and confirmed by product ion spectra library matching, taking into account product ions exact mass and intensities. One-hundred pi, urine was subjected to solid phase cation exchange extraction (SOLA SCX). The chromatographic reverse-phase separation was achieved with gradient mobile phase of 0.1% formic acid in water and in acetonitrile in 20 min. The assay was linear from 2.5 or 5 to 500 mu g/L. Imprecision (n = 15) was less than15.4%, and accuracy (n = 15) 84.2-118.5%. Extraction efficiency was 51.2-111.2%, process efficiency 57.7-104.9% and matrix effect ranged from -41.9% to 238.5% (CV less than 23.3%, except MDBZP CV less than 34%). Authentic urine specimens (n = 62) were analyzed with the method that provides a comprehensive confirmation for 40 new stimulant drugs with specificity and sensitivity.

  • 4.
    Jonsson, Susanne
    et al.
    Linköping University, The Tema Institute, Department of Water and Environmental Studies. Linköping University, Faculty of Arts and Sciences.
    Borén, Hans
    Linköping University, Department of Physics, Chemistry and Biology, Organic Analytical Chemistry. Linköping University, The Institute of Technology.
    Analysis of mono- and diesters of o-phthalic acid by solid-phase extractions with polystyrene–divinylbenzene-based polymers2002In: Journal of Chromatography A, ISSN 0021-9673, E-ISSN 1873-3778, Vol. 963, no 1-2, p. 393-400Article in journal (Refereed)
    Abstract [en]

    Retention mechanisms of an unmodified and a hydroxylated polystyrene–divinylbenzene polymer were studied by solid-phase extraction of o-phthalic acid and some of its mono- and diesters from purified water and then analysing by GC–MS. The monoesters and phthalic acid were retained only when protonated (i.e. acidified with HCl to pH 0.9). Of all elution solvents tested, ethyl acetate gave the best overall recoveries (61–89%) with both polymers. Applicability to complex matrixes (e.g. acidogenic landfill leachates) was examined by introducing a washing step with acetone in acidified water (pH 0.9) to eliminate volatile fatty acids (C2–C6) from the cartridge. Finally, the method was tested on real samples.

  • 5.
    Jonsson, Susanne
    et al.
    Linköping University, The Tema Institute, Department of Water and Environmental Studies. Linköping University, Faculty of Arts and Sciences.
    Nielsen, Annika T.
    Linköping University, The Tema Institute, Department of Water and Environmental Studies. Linköping University, Faculty of Arts and Sciences.
    Quantification of volatile sulfur compounds in complex gaseous matrices by solid-phase microextraction2002In: Journal of Chromatography A, ISSN 0021-9673, E-ISSN 1873-3778, Vol. 963, no 1-2, p. 57-64Article in journal (Refereed)
    Abstract [en]

    Procedures were assessed for quantifying nine volatile sulfur compounds found in complex gaseous samples collected at a biogas-production plant and a sewage treatment plant. The target compounds were extracted by solid-phase microextraction (using the 75-╡m Carboxen-polydimethylsiloxane fiber coating) at 22░C for 20 min, and analyzed by GC-MS. Detection limits ranged between 1 pptv (v/v) for carbon disulfide and 470 pptv (v/v) for hydrogen sulfide. High amounts of organic compounds were found during full-scan analysis of the samples and standard additions to individual sub-samples revealed that the analysis was subject to matrix effects. However, the functions obtained by standard additions were still linear and quantification was possible for all the compounds tested except hydrogen sulfide. No detectable losses were observed during storage in the sampling containers, made of Tedlar film, over a storage period of 20 h. However, water permeated through the walls and the relative humidity in the bag increased during storage until it reached the ambient level. Finally, it was shown that the drying agent, CaCl2, caused no detectable losses of any of the compounds. ⌐ 2002 Elsevier Science B.V. All rights reserved.

  • 6.
    Josefsson, Martin
    et al.
    National Board of Forensic Medicine.
    Sabanovic, A
    National Board of Forensic Medicine.
    Sample preparation on polymeric solid phase extraction sorbents for liquid chromatographic-tandem mass spectrometric analysis of human whole blood - A study on a number of beta-agonists and beta-antagonists2006In: Journal of Chromatography A, ISSN 0021-9673, E-ISSN 1873-3778, Vol. 1120, no 02-Jan, p. 1-12Article in journal (Refereed)
    Abstract [en]

    Alternative strategies for sample preparation of human blood samples were evaluated including protein precipitation (PP) and solid phase extraction (SPE) on Waters Oasis® polymeric columns. Gradient chromatography within 15 min was performed on a Hypersil Polar-RP column combined with a Sciex API 2000 triple quadrupol instrument equipped with an electro-spray interface. Beta-agonists and beta-antagonists available on the Swedish market were included in the study. A combination of zinc sulphate and ethanol was found effective for PP. A clear supernatant was achieved that either could be injected directly on the LC–MS–MS system for analysis or transferred to a SPE column for further extraction and analyte concentration. Retention on the hydrophilic–lipophilic balanced sorbent HLB as well as the mixed mode cationic MCX and anionic MAX sorbents were investigated. On HBL the relative lipophilicity of the target analytes was investigated. At a high pH when the amino alcohols are deprotonised the more non-polar analytes (e.g., carvediol, betaxolol, bisoprolol and propranolol) were well retained on the sorbent and for the majority methanol content higher than 50% in water (v/v) was needed for elution. Some analytes though, with additional weak acidic functionalities (fenoterol, salbutamol, sotalol, and terbutaline) were poorly retained. On MAX the retention of these weak acids was improved when loaded under basic conditions but under neutral conditions analyte recoveries was comparable with HLB. On MCX all the analytes were well retained allowing a wash step of 100% methanol at neutral and low pH. By applying the supernatant from PP in combination with an additional portion of aqueous formic acid (2%) the analytes could be loaded and retained. High extraction recoveries were found for most analytes but for a few, significant losses were seen during PP (e.g., formoterol) and/or evaporation (e.g., fenoterol, formoterol, labetalol and terbutaline). The effectiveness of the sample preparation was evaluated by ESI ion-suppression studies by post column infusion of the target analyte. An ethanol zinc sulphate aq mixture was found to be more effective than acetonitrile, methanol or ethanol for PP of human whole blood samples. Beside suppression by salts in the front peak, only limited suppression from other artefacts such as more lipophilic compounds was found late in the chromatograms. Some tendency though to concentrate more lipophilic artefacts on the Oasis® sorbents was seen. These findings show that the Oasis MCX sorbent is well suited for sample preparation of beta-agonists and beta-antagonists from human whole blood if the objective is to cover a great number of the analytes in the same assay.

  • 7. Lagesson, V.
    et al.
    Lagesson-Andrasko, L.
    Andrasko, J.
    Baco, F.
    Baco, F..
    Identification of compounds and specific functional groups in the wavelength region 168-330 nm using gas chromatography with UV detection2000In: Journal of Chromatography A, ISSN 0021-9673, E-ISSN 1873-3778, Vol. 867, no 1-2, p. 187-206Article in journal (Refereed)
    Abstract [en]

    A GC-UV instrumental set up with two different GC units has been used for determination of specific functional groups and compounds in complex mixtures. Separations have been made using a micro gas chromatograph built into a gas flow cell and by means of an external capillary gas chromatograph linked to the same gas flow cell. Four various applications (cigarette smoke, petroleum, dust, flavour) have been performed in order to demonstrate the potential of the GC-UV method. Gas phase UV spectra have been recorded in the region of 168-330 nm. Based on a gas phase spectrum reference library the identification of unknowns as well as the determination of specific functional groups have been achieved. A table showing the spectral shapes and positions of the absorption bands for 50 specific functional groups is presented. The advantage of using derivative spectra in order to amplify spectral details and improve selectivity is discussed. Regarding sensitivity, it has been found that identifications can be made in the mid-pg range and limit of detection for naphthalenes are at a level of 0.5-3 pg/s. Copyright (C) 2000 Elsevier Science B.V.

  • 8.
    Landberg, Eva
    et al.
    Linköping University, Department of Biomedicine and Surgery, Clinical Chemistry. Linköping University, Faculty of Health Sciences.
    Lundblad, Arne
    Linköping University, Department of Biomedicine and Surgery, Clinical Chemistry. Linköping University, Faculty of Health Sciences.
    Påhlsson, Peter
    Linköping University, Department of Biomedicine and Surgery, Clinical Chemistry. Linköping University, Faculty of Health Sciences.
    Temperature effects in high-performance anion-exchange chromatography of oligosaccharides1998In: Journal of Chromatography A, ISSN 0021-9673, E-ISSN 1873-3778, Vol. 814, no 1-2, p. 97-104Article in journal (Refereed)
    Abstract [en]

    High-performance anion-exchange chromatography (HPAEC) with pulsed amperometric detection has been widely used for analysis of mono-, oligo- and polysaccharides. Many factors that affect separation of carbohydrates by HPAEC have been evaluated, however effect of temperature has not been carefully studied. In the present study, neutral and sialylated oligosaccharides from human milk and different types of N-linked oligosaccharides were analysed by HPAEC at temperatures ranging from 13 to 30°C. N-Acetyl neuraminic acid, galacturonic acid and stachyose were also analysed since they have been used as internal standards when analysing various oligosaccharides by HPAEC. All oligosaccharides showed decreased retention times with increased temperature. Even small differences in temperature (i.e. ±5°) resulted in considerable changes in retention times. In addition, individual oligosaccharides showed different relative changes in retention time with increased temperature. By changing the temperature, a switch in elution order of individual oligosaccharides were sometimes found. These results show that retention times relative to an internal standard cannot be used for oligosaccharide identification unless temperature is carefully controlled. Regulation of temperature is also a valuable tool in achieving optimal separation of oligosaccharides by HPAEC.

  • 9.
    Nezirevic Dernroth, Dzeneta
    et al.
    Linköping University, Department of Clinical and Experimental Medicine, Clinical Chemistry. Linköping University, Faculty of Health Sciences. Östergötlands Läns Landsting, Centre for Laboratory Medicine, Department of Clinical Chemistry.
    Rundström, Annica
    Linköping University, Department of Clinical and Experimental Medicine, Clinical Chemistry. Linköping University, Faculty of Health Sciences.
    Kågedal, Bertil
    Linköping University, Department of Clinical and Experimental Medicine, Clinical Chemistry. Linköping University, Faculty of Health Sciences. Östergötlands Läns Landsting, Centre for Laboratory Medicine, Department of Clinical Chemistry.
    Gas chromatography-mass spectrometry analysis of pheomelanin degradation products2009In: Journal of Chromatography A, ISSN 0021-9673, E-ISSN 1873-3778, Vol. 1216, no 30, p. 5730-5739Article in journal (Refereed)
    Abstract [en]

    Melanoma is most rapidly increasing in the white population and people with pheomelanin skin type are at high risk to develop melanoma. However, little is known about the pheomelanin structure and function, and further elucidation of this melanin is therefore an important task. A GC/MS method was developed based on hydriodic acid hydrolysis of pheomelanin in the urine. Derivatization was performed with ethyl chloroformate and ethanol:pyridine (4:1, v/v). N,O-Ethoxycarbonyl-ethyl esters were extracted with chloroform and analyzed by GC/MS. 4-Amino-3-hydroxyphenylaianine and 3-amino4-hydroxyphenylaianine together with one benzothiazinone and two benzothiazole compounds were detected and identified in hydrolyzed samples of synthetic pheomelanin and melanin from the urine of a patient with melanoma. These findings strongly suggest that heterocyclic pheomelanin-type units are incorporated in the pigment structures.

  • 10.
    Nezirevic Dernroth, Dzeneta
    et al.
    Linköping University, Faculty of Health Sciences. Linköping University, Department of Biomedicine and Surgery, Division of clinical chemistry.
    Årstrand, Kerstin
    Linköping University, Faculty of Health Sciences. Linköping University, Department of Biomedicine and Surgery, Division of clinical chemistry.
    Kågedal, Bertil
    Linköping University, Faculty of Health Sciences. Linköping University, Department of Biomedicine and Surgery, Division of clinical chemistry.
    Hydrophilic interaction liquid chromatographic analysis of aminohydroxyphenylalanines from melanin pigments2007In: Journal of Chromatography A, ISSN 0021-9673, E-ISSN 1873-3778, Vol. 1163, no 1-2, p. 70-79Article in journal (Refereed)
    Abstract [en]

    Malignant melanomas are more often seen in subjects with light colored skin who tan poorly than in persons who tan more rapidly. This has been attributed to the structure of their pigment, pheomelanin, which differs markedly from the eumelanin of persons with darker skin. To study the hydrolysis products of pheomelanin pigments a new method was developed for analysis of 4-amino-3-hydroxyphenylalanine (4-AHP) and 3-amino-4-hydroxyphenylalanine (3-AHP). Pheomelanin samples were hydrolyzed and extracted with solid-phase extraction columns using strong cation-exchange (SCX) cartridges. Separation of 4-AHP and 3-AHP was achieved on a ZIC-HILIC column (150 mm × 2.1 mm I.D.) with a mobile phase consisting of acetonitrile:0.1 M ammonium acetate buffer, pH 4.5 (82:18, v/v). Detection was performed with an electrochemical detector at +400 mV. Run time was 30 min. The limits of detection were 73 pg and 51 pg for 4-AHP and 3-AHP respectively, using 2 μl injections. Good linearity was found within the range 0.05-5.0 μg/ml. Absolute recovery was 70% and relative recovery was 100%. The AHPs were stable for 1 year in the hydrolyzed samples, for 4 days in the eluates from solid-phase sorbents stored in the refrigerator, and for 2 days diluted with mobile phase and stored in the autosampler at 10 °C. The within-day imprecision was <5% and the between-day imprecision was <7% for the two analytes. The method, applied to the analysis of pheomelanin in urine from human melanoma patients, allows the analysis of 30 samples in one set and is suitable for routine work with human hair and melanoma cells. By using the ZIC-HILIC stationary phase, ion-pairing reagents could be avoided, which makes the method suitable to further analysis of degradation products from pheomelanins using mass spectrometric detection. © 2007 Elsevier B.V. All rights reserved.

  • 11.
    Shamshir, Adel
    et al.
    Umea Univ, Sweden.
    Phuoc Dinh, Ngoc
    Diduco AB, Sweden.
    Jonsson, Tobias
    Diduco AB, Sweden.
    Sparrman, Tobias
    Umea Univ, Sweden.
    Ashiq, Muhammad Jamshaid
    Umea Univ, Sweden.
    Irgum, Knut
    Umea Univ, Sweden.
    Interaction of toluene with polar stationary phases under conditions typical of hydrophilic interaction chromatography probed by saturation transfer difference nuclear magnetic resonance spectroscopy2019In: Journal of Chromatography A, ISSN 0021-9673, E-ISSN 1873-3778, Vol. 1588, p. 58-67Article in journal (Refereed)
    Abstract [en]

    Toluene has been used as void volume (zero retention) marker since the inception of hydrophilic interaction chromatography (HILIC), based on the assumption that its hydrophobicity should prevent it from interacting with stationary phases envisioned to be covered by relatively thick layers of water. Recent work has shown that the void volumes of partly water-swollen HILIC phases are not identical to the volumes probed by toluene, yet the compound is still ubiquitously used as void volume marker. As part of our investigations of the retention mechanisms in HILIC, we probed the extent to which toluene is capable of penetrating into the water-enriched layer and to interact with the functional groups of three commercially available hydrophilic and polar stationary phases with different charge properties and water-retaining abilities, using saturation transfer difference H-1 nuclear magnetic resonance (STD-NMR) spectroscopy at high resolution magic angle spinning (HR-MAS) conditions. The test solutions were 1000 ppm of toluene in deuterated acetonitrile and water mixtures, with and without addition of ammonium acetate, in order to mimic a set of conditions typically encountered in HILIC separations. Interactions between toluene and the functional groups on the stationary phases were probed by equilibrating the phases with these eluent mimics and measuring the transfer of magnetization from stationary phase protons to the protons of toluene. Our results show that toluene is indeed capable of traversing the water-enriched layers of all the three tested phases and of interacting with protons that are tightly associated with the stationary phases. (C) 2018 Published by Elsevier B.V.

  • 12.
    Vikingsson, Svante
    et al.
    Linköping University, Department of Medical and Health Sciences, Clinical Pharmacology. Linköping University, Faculty of Health Sciences.
    Kronstrand, Robert
    Linköping University, Department of Medical and Health Sciences, Division of Drug Research. Linköping University, Faculty of Health Sciences.
    Josefsson, Martin
    Department of Forensic Genetics and Forensic Toxicology, National Board of Forensic Medicine, Artillerigatan 12, SE-581 33 Linköping, Sweden.
    Retention of opioids and their glucuronides on a combined zwitterion and hydrophilic interaction stationary phase2008In: Journal of Chromatography A, ISSN 0021-9673, E-ISSN 1873-3778, Vol. 1187, no 01-Feb, p. 46-52Article in journal (Refereed)
    Abstract [en]

    A stationary phase combining zwitterionic ion chromatography and hydrophilic interaction chromatography (ZIC-HILIC) from SeQuant was evaluated for the chromatography of some opiates and their polar metabolites. The effects of mobile phase constitution on retention and resolution were extensively evaluated. Different aspects of mobile phase constitution such as ion strength and type of buffer, type and amount of organic modifier and pH were examined. The selectivity and retention of the opiates compared to their glucuronides could be substantially altered with small changes of the mobile phase, especially when the type of buffer, i.e., formate, or acetate and organic modifier, i.e., acetonitrile or methanol were changed. The retention on the ZIC-HILIC was dominated by hydrophilic interaction chromatography (HILIC) but considerable effects on the selectivity was observed, possibly caused by an ion exchange mechanism due to interactions with the charges on the stationary phase.

  • 13.
    Öhman, Daniel
    et al.
    Linköping University, Department of Medicine and Care, Clinical Pharmacology. Linköping University, Faculty of Health Sciences.
    Norlander, Björn
    Linköping University, Department of Medicine and Care, Clinical Pharmacology. Linköping University, Faculty of Health Sciences.
    Peterson, Curt
    Linköping University, Department of Medicine and Care, Clinical Pharmacology. Linköping University, Faculty of Health Sciences.
    Bengtsson, Finn
    Linköping University, Department of Medicine and Care, Clinical Pharmacology. Linköping University, Department of Neuroscience and Locomotion, Psychiatry. Linköping University, Faculty of Health Sciences.
    Simultaneous determination of reboxetine and O-desethylreboxetine enantiomers using enantioselective reversed-phase high-performance liquid chromatography2002In: Journal of Chromatography A, ISSN 0021-9673, E-ISSN 1873-3778, Vol. 947, no 2, p. 247-254Article in journal (Refereed)
    Abstract [en]

    Current knowledge of stereoselective pharmacokinetics and different potencies of drug enantiomers requires the performance of stereoselective analysis during therapeutic drug monitoring in clinical practice. However, in the case of the new antidepressant drug reboxetine, no effort has been made so far to find a such a suitable system. Therefore, as a step towards developing an enantioselective bioanalytical method for reboxetine and the O-desethylreboxetine metabolite, three stereoselective chromatographic approaches have been investigated. Several chiral columns were tested, among them Chiral-AGP, ChiraGrom 2 and Chiral-CBH, which were able to simultaneously separate the two compounds into enantiomers in total running times of 28, 18 and 12 min, respectively.

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