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  • 1.
    Abdel-Rehim, Mohamed
    Stockholm University, Faculty of Science, Department of Analytical Chemistry.
    Microextraction by packed sorbent (MEPS): A tutorial2011In: Analytica Chimica Acta, ISSN 0003-2670, E-ISSN 1873-4324, Vol. 701, no 2, p. 119-128Article in journal (Refereed)
    Abstract [en]

    This tutorial provides an overview on a new technique for sample preparation, microextraction by packed sorbent (MEPS). Not only the automation process by MEPS is the advantage but also the much smaller volumes of the samples, solvents and dead volumes in the system. Other significant advantages such as the speed and the simplicity of the sample preparation process are provided. In this tutorial the main concepts of MEPS will be elucidated. Different practical aspects in MEPS are addressed. The factors affecting MEPS performance will be discussed. The application of MEPS in clinical and pre-clinical studies for quantification of drugs and metabolites in blood, plasma and urine will be provided. A comparison between MEPS and other extraction techniques such as SPE, LLE, SPME and SBSE will be discussed.

  • 2.
    Ahmadi, Mazaher
    et al.
    Stockholm University, Faculty of Science, Department of Environmental Science and Analytical Chemistry. Bu-Ali Sina University, Iran.
    Elmongy, Hatem
    Stockholm University, Faculty of Science, Department of Environmental Science and Analytical Chemistry.
    Madrakian, Tayyebeh
    Abdel-Rehim, Mohamed
    Stockholm University, Faculty of Science, Department of Environmental Science and Analytical Chemistry.
    Nanomaterials as sorbents for sample preparation in bioanalysis: A review2017In: Analytica Chimica Acta, ISSN 0003-2670, E-ISSN 1873-4324, Vol. 958, p. 1-21Article, review/survey (Refereed)
    Abstract [en]

    In recent years, application of nanomaterials as sorbent has gained the attention of researchers in bioanalysis. Different nanomaterials have been utilized as the sorbent in extraction techniques such as solid phase extraction, dispersive solid phase extraction, magnetic solid phase extraction, microextraction by packed sorbent, solid phase microextraction, dispersive pt-solid phase extraction, and stir bar sorptive extraction. In the present review, different nanomaterials which have recently been utilized as sorbent for bioanalysis are classified into six main groups, namely metallic, metallic and mixed oxide, magnetic, carbonaceous, silicon, and polymer-based nanomaterials. Application of these nanomaterials in different extraction techniques for bioanalysis has been reviewed. This study shows that magnetic nanomaterials have gained significant attention owing to their magnetic separation ability. In addition, the present review shows that there is a lack in the application of nanomaterials for on-line analysis procedures, most probably due to some intrinsic properties of nanomaterials such as spontaneous agglomeration.

  • 3.
    El-Beqqali, Aziza
    et al.
    Stockholm University, Faculty of Science, Department of Environmental Science and Analytical Chemistry.
    Abdel-Rehim, Mohamed
    Stockholm University, Faculty of Science, Department of Environmental Science and Analytical Chemistry.
    Molecularly imprinted polymer-sol-gel tablet toward micro-solid phase extraction: I. Determination of methadone in human plasma utilizing liquid chromatography-tandem mass spectrometry2016In: Analytica Chimica Acta, ISSN 0003-2670, E-ISSN 1873-4324, Vol. 936, p. 116-122Article in journal (Refereed)
    Abstract [en]

    In the present work molecularly imprinted sol-gel tablet (MIP-Tablet) was prepared. The MIP-sol-gel was prepared as a thin layer on polyethylene material in a tablet form. Methadone-d9 was selected as the template and 3-(propylmethacrylate)-trimethoxysilane was used as precursor. MIP-Tablet was applied for micro-solid phase extraction (μ-SPE). The MIP-Tablet was used for the determination of methadone in human plasma samples utilizing liquid chromatography-tandem mass spectrometry; and each tablet could be used twenty times. The extraction time was 10 min while desorption time was 6 min. Factors affecting the extraction efficiency such as desorption solvents, sample pH, salt addition, extraction time, desorption time and adsorption capacity were investigated. The calibration curves were obtained within the range of 5-5000 ng/mL using methadone in human plasma samples. The coefficients of determination (r(2)) values were >= 0.999 for all runs and the extraction recovery was >80%. The accuracy values for quality control samples varied from +3.6 to +9.7% and the inter-day precision (RSD %) values were ranged from 5.0 to 8.0%. The limit of detection was 1.0 ng/mL and the lower limit of quantification was 5 ng/mL utilizing methadone in human plasma samples.

  • 4.
    Gao, Qiuju
    et al.
    Stockholm University, Faculty of Science, Department of Meteorology .
    Araia, Musie
    Leck, Caroline
    Stockholm University, Faculty of Science, Department of Meteorology .
    Emmer, Åsa
    Characterization of exopolysaccharides in marine colloids by capillary electrophoresis with indirect UV detection2010In: Analytica Chimica Acta, ISSN 0003-2670, E-ISSN 1873-4324, Vol. 662, no 2, p. 193-199Article in journal (Refereed)
    Abstract [en]

    A method was established using capillary electrophoresis with indirect UV detection for analysis of monosaccharides liberated from exopolysaccharides by acidic hydrolysis. Tangential flow filtration was used to isolate high molecular weight polysaccharides from seawater. The capillary electrophoresis method included the use of a background electrolyte consisting of 2,6-dimethoxyphenol and cetyltrimethylammonium bromide. Several neutral sugars commonly existing in marine polysaccharides were separated under optimized conditions. The relative standard deviations were between 1.3% and 2.3% for relative migration time and 1.3-2.5% for peak height. Detection limits (at S/N 3) were in the range of 27.2-47.8 mu M. The proposed approach was applied to the analysis of hydrolyzed colloidal polysaccharides in seawater collected from the Baltic Sea. Nanomolar levels of liberated monosaccharides in seawater samples can be detected by preconcentration up to 30,000 times.

  • 5. Kubán, P
    et al.
    Karlberg, B
    Stockholm University, Faculty of Science, Department of Analytical Chemistry.
    Flow/sequential injection sample treatment coupled to capillary electrophoresis. A review2009In: Analytica Chimica Acta, ISSN 0003-2670, E-ISSN 1873-4324, Vol. 648, p. 129-145Article in journal (Refereed)
    Abstract [en]

    Various flow sample handling approaches coupled to capillary electrophoresis (CE) are reviewed, covering the research in this field in the 12 years since the milestone year of 1997, when practical interfaces to on-line couple flow injection (FI) and capillary electrophoresis were first developed independently by two research groups. Some previous attempts are also presented. Since 1997 a plethora of ingenious coupled systems have been developed. Although several reviews are available on various aspects of the topic, we have opted for a comprehensive overview of all FI-CE systems, as well as related and similar systems. This coupling has thus also led to the development of systems based on hybrids between the classical and microchip approaches. Truly microchip FI-CE systems are also included in this review. The developed systems have been used for various sample treatments, including on-line membrane-assisted sample treatment, column-based preconcentration, on-line derivatization and monitoring, to name just a few. The utility of coupling flow sampling to CE has been demonstrated in various practical applications that are discussed in detail. The current state-of-the-art and foreseeable future developments are also discussed.

  • 6.
    Li, Zhe
    et al.
    Stockholm University, Faculty of Science, Department of Applied Environmental Science (ITM).
    Maier, Michael P.
    Radke, Michael
    Stockholm University, Faculty of Science, Department of Applied Environmental Science (ITM).
    Screening for pharmaceutical transformation products formed in river sediment by combining ultrahigh performance liquid chromatography/high resolution mass spectrometry with a rapid data-processing method2014In: Analytica Chimica Acta, ISSN 0003-2670, E-ISSN 1873-4324, Vol. 810, p. 61-70Article in journal (Refereed)
    Abstract [en]

    While the occurrence of pharmaceuticals in the aquatic environment has been extensively investigated, their environmental fate is less thoroughly explored. Scarce information on their transformation pathways and transformation products (TPs) limits conventional target analytical approaches. In this study, samples from water/sediment tests were analyzed by ultrahigh performance liquid chromatography interfaced with quadrupole time-of-flight mass spectrometry (UHPLC/QToF-MS). A data processing method based on peak detection, time-trend filtration and structure assignment was established to provide an efficient way for identifying the key TPs in terms of persistence; all software used for the individual steps of this method is freely available. The accurate mass and meaningful time-trends were major contributors in facilitating the isolation of plausible TP peaks. In total, 16 TPs from 9 parent pharmaceuticals were identified. Eleven out of the 16 TPs were confirmed by corresponding reference standards; no standards were available for the remaining TPs. For additional 6 potential TPs, a molecular formula was suggested but no additional structural information could be generated. Among the TPs identified in the water/sediment tests, carbamazepine-10,11-epoxide (parent: carbamazepine), saluamine (parent: furosemide), chlorothiazide and 4-amino-6-chloro-1,3-benzenedisulfonamide (parent of both: hydrochlorothiazide), and 1-naphthol (parent: propranolol) accumulated over the entire incubation period of 35 days.

  • 7.
    Marand, Åsa
    et al.
    Stockholm University, Faculty of Science, Department of Analytical Chemistry.
    Karlsson, Daniel
    Stockholm University, Faculty of Science, Department of Analytical Chemistry.
    Dalene, Marianne
    Stockholm University, Faculty of Science, Department of Analytical Chemistry.
    Skarping, Gunnar
    Stockholm University, Faculty of Science, Department of Analytical Chemistry.
    Extractable organic compounds in polyurethane foam with special reference to aromatic amines and derivatives thereof2004In: Analytica Chimica Acta, ISSN 0003-2670, E-ISSN 1873-4324, Vol. 510, no 1, p. 109-119Article in journal (Refereed)
    Abstract [en]

    Methods for determination of aromatic amines and related compounds in flexible toluene diisocyanate (TDI)-based polyurethane (PUR) foam were investigated. The foam was extracted using 0.1% (w/v) aqueous acetic acid (HAc). Extraction solutions were analysed and aromatic amines were determined as ethyl chloroformate (Et) and pentafluoropropionic acid anhydride (PFPA) derivatives. The determinations were performed using liquid chromatography (LC) and mass spectrometry (MS) detection with electrospray ionisation (ESI) or gas chromatography (GC)-MS with chemical ionisation monitoring negative ions (NCI). The Et derivatives were determined using LC-ESI+-MS with detection limit of 2 pg of toluenediamine (TDA). The PFPA derivatives were determined using LC-ESI--MS or GC-NCI-MS with detection limits of 0.1 and 0.02 pg of TDA, respectively. Using trideuterium labelled TDA as internal standard, linear calibration curves were obtained in the range of 0.01-0.50 mug ml(-1) (n = 7), with correlation coefficients >0.999. When plotting calibration curves for TDA-PFPA derivatives determined using LC-MS against TDA-PFPA using GC-MS and TDA-Et using LC-MS, linear curves were obtained. The relative standard deviation (R.S.D.) for determination of TDA in foam extraction solutions were 13%. LC-MS determination of PFPA derivatives was more selective, as compared to LC-MS of Et derivatives.

    In foam extraction solutions, 2,4- and 2,6-TDA, several isomers of methylenedianiline (MDA) and dimers of TDA/TDI were observed. 2,4-TDA and 4,4'-MDA are possible human carcinogens. Hydrolysis of the extraction solution revealed a large pool of TDA/TDI compounds and oligomers. The concentration of TDA in foam was affected by the extraction media, temperature and duration. The choice of derivatisation procedure also affected the determination of TDA. In extraction solutions from six different commercially available flexible foam qualities 2,4- and 2,6-TDA were found in the range of 0-7 and 0-6 mug g(-1) foam, respectively. When flexible foam was heated, considerable higher concentrations of TDA were observed.

  • 8.
    Riboni, Nicolò
    et al.
    Università di Parma, Italy.
    Magrini, Laura
    Bianchi, Federica
    Careri, Maria
    Cappiello, Achille
    Sol-gel coated ion sources for liquid chromatography-direct electronionization mass spectrometry2017In: Analytica Chimica Acta, ISSN 0003-2670, E-ISSN 1873-4324, Vol. 978, p. 35-41Article in journal (Refereed)
    Abstract [en]

    Advances in interfacing liquid chromatography and electron ionization mass spectrometry are presented. New ion source coatings synthesized by sol-gel technology were developed and tested as vaporization surfaces in terms of peak intensity, peak width and peak delay for the liquid chromatography-direct electron ionization mass spectrometry (Direct-EI) determination of environmental pollutants like polycyclic aromatic hydrocarbons and steroids. Silica-, titania-, and zirconia-based coatings were sprayed inside the stainless steel ion source and characterized in terms of thermal stability, film thickness and morphology. Negligible weight losses until 350–400 °C were observed for all the materials, with coating thicknesses in the 6 (±1)-11 (±2) μm range for optimal ionization process. The best performances in terms of both peak intensity and peak width were obtained by using the silica-based coating: the detection of the investigated compounds was feasible at low ng μl−1 levels with a good precision (RSD < 9% for polycyclic aromatic hydrocarbons and <11% for hormones).

  • 9.
    Riboni, Nicolò
    et al.
    Università degli Studi di Parma, Italy.
    Trzcinski, Jakub W.
    Bianchi, Federica
    Massera, Chiara
    Pinalli, Roberta
    Sidisky, Leonard
    Dalcanale, Enrico
    Careri, Maria
    Conformationally blocked quinoxaline cavitand as solid-phase microextraction coating for the selective detection of BTEX in air2016In: Analytica Chimica Acta, ISSN 0003-2670, E-ISSN 1873-4324, Vol. 905, p. 79-84Article in journal (Refereed)
    Abstract [en]

    A tetraquinoxaline cavitand functionalized with methylenoxy bridges at the upper rim is proposed as selective solid-phase microextraction (SPME) coating for the determination of BTEX at trace levels in air. The SPME fibers were characterized in terms of film thickness, morphology, thermal stability and extraction capabilities. An average coating thickness of 35 (±4) μm, a thermal stability up to 350 °C and a good fiber-to-fiber and batch-to-batch repeatability with RSD lower than 15% were obtained. Excellent enrichment factors ranging from 360–700 × 103 were obtained for the investigated compounds. Finally, method validation proved the capabilities of the developed coating for the selective sampling of BTEX, achieving LOD values in the 0.4–1.2 ng m−3 range.

  • 10.
    Riddar, Jakob Johnson
    et al.
    Stockholm University, Faculty of Science, Department of Analytical Chemistry.
    Karlsson, Daniel
    Stockholm University, Faculty of Science, Department of Analytical Chemistry.
    Dalene, Marianne
    Stockholm University, Faculty of Science, Department of Analytical Chemistry.
    Skarping, Gunnar
    Stockholm University, Faculty of Science, Department of Analytical Chemistry.
    Determination of aromatic amines in aqueous extracts of polyurethane foam using hydrophilic interaction liquid chromatography and mass spectrometry2010In: Analytica Chimica Acta, ISSN 0003-2670, E-ISSN 1873-4324, Vol. 678, no 1, p. 117-123Article in journal (Refereed)
    Abstract [en]

    A method is presented for the determination of aromatic amines in aqueous extracts of polyurethane (PUR) foam. The method is based on the extraction of PUR foam using aqueous acetic acid (0.1%, w/v) followed by determination of extracted aromatic amines using hydrophilic interaction liquid chromatography (HILIC) and tandem mass spectrometry (MS/MS) with positive electrospray ionisation. The injections of volumes up to 5 mu L of aqueous solutions were made possible by on-column focusing with partially filled loop injections. The fragmentation patterns for 2,4- and 2,6-toluene diamine (TDA) and 4,4'-methylene dianiline (MDA) were clarified by performing a hydrogen-deuterium exchange study. TDA and MDA were determined using trideuterated 2,4- and 2,6-TDA and dideuterated 4,4'-MDA as internal standards. Linear calibration graphs were obtained over the range 0.025-0.5 mu g mL(-1) with correlation coefficients >0.996 and the instrumental detection limit for each compound was <50 fmol. The stability of the amines was influenced by the matrix, so their concentrations decreased over time. Agreement was observed between the results of analyses of PUR foam extracts by HILIC-MS/MS and results obtained by ethyl chloroformate derivatisation and reversed phase (RP) liquid chromatography-mass spectrometry (LC-MS/MS). TDA was observed to be unstable in extracts of foam but not in pure solutions.

  • 11.
    Wiberg, Kent
    et al.
    Stockholm University, Faculty of Science, Department of Analytical Chemistry.
    Jacobsson, Sven P.
    Stockholm University, Faculty of Science, Department of Analytical Chemistry.
    Parallel factor analysis of HPLC-DAD data for binary mixtures of lidocaine and prilocaine with different levels of separation2004In: Analytica Chimica Acta, ISSN 0003-2670, E-ISSN 1873-4324, Vol. 514, no 2, p. 203-209Article in journal (Refereed)
    Abstract [en]

    A set of 17 samples containing a constant amount of lidocaine (667 muM) and a decreasing amount of prilocaine (667-0.3 muM) was analysed by LC-DAD at three different levels of separation, followed by parallel factor analysis (PARAFAC) of the data obtained. In Case 1 no column was connected, the chromatographic resolution (R-s) therefore being zero, while Cases 2 and 3 had partly separated peaks (R-s = 0.7 and 1.0). The results showed that in Case 1, analysed without any separation, the PARAFAC decomposition with a model consisting of two components gave a good estimate of the spectral and concentration profiles of the two compounds. In Cases 2 and 3, the use of PARAFAC models with two components resolved the underlying chromatographic, spectral and concentration profiles. The loadings related to the concentration profile of prilocaine were used for regression and prediction of the prilocaine content. The results showed that prediction of prilocaine content was possible with satisfactory prediction (RMSEP < 0.01). This study shows that PARAFAC is a powerful technique for resolving partly separated peaks into their pure chromatographic, spectral and concentration profiles, even with completely overlapping spectra and the absence or very low levels of separation.

  • 12.
    Yuan, Bo
    et al.
    Stockholm University, Faculty of Science, Department of Environmental Science and Analytical Chemistry.
    Muir, Derek
    MacLeod, Matthew
    Stockholm University, Faculty of Science, Department of Environmental Science and Analytical Chemistry.
    Methods for trace analysis of short-, medium-, and long-chain chlorinated paraffins: Critical review and recommendations2019In: Analytica Chimica Acta, ISSN 0003-2670, E-ISSN 1873-4324, Vol. 1074, p. 16-32Article, review/survey (Refereed)
    Abstract [en]

    Many methods for quantifying chlorinated paraffins (CPs) yield only a total concentration of the mixture as a single value. With appropriate analytical instrumentation and quantification methods, more reliable and detailed analysis can be performed by quantifying total concentrations of short-, medium-, and longchain CPs (SCCPs, MCCPs, and LCCPs), and in the current optimal situation by quantifying individual carbon-chlorine congener groups (CnClm). Sample extraction and clean-up methods for other persistent organochlorines that have been adapted for recovery of CPs must be applied prior to quantification with appropriate quality assurance and quality control to ensure applicability of the methods for SCCPs, MCCPs, and LCCPs. Part critical review, part tutorial, and part perspective, this paper provides practical guidance to analytical chemists who are interested in establishing a method for analysis of CPs in their lab facilities using commercial reference standards, or for expanding existing analysis of total CPs or SCCPs to analysis of SCCPs, MCCPs, and LCCPs, or to analysis of CnClm congener groups.

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