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  • 1. Batlle, R
    et al.
    López, P
    Nerín, C
    Crescenzi, C
    Stockholm University, Faculty of Science, Department of Analytical Chemistry.
    Active single-drop microextraction for the determination of gaseous diisocyanates2008In: Journal Of Chromatography A, Vol. 1185, p. 155-160Article in journal (Refereed)
  • 2.
    Crescenzi, C
    et al.
    Stockholm University, Faculty of Science, Department of Analytical Chemistry.
    Albinana, J
    Carlsson, H
    Holmgren, E
    Batlle, R
    On-line strategies for determining trace levels of nitroaromatic explosives and related compounds in water2007In: J. Chromatogr. A, Vol. 1153, no 1-2, p. 186-193Article in journal (Refereed)
  • 3.
    Iadaresta, Francesco
    et al.
    Stockholm University, Faculty of Science, Department of Environmental Science and Analytical Chemistry.
    Avagyan, Rozanna
    Strzałka, Emilia
    Crescenzi, Carlo
    Stockholm University, Faculty of Science, Department of Environmental Science and Analytical Chemistry.
    Östman, Conny
    Stockholm University, Faculty of Science, Department of Environmental Science and Analytical Chemistry.
    Determination of Textile Related Compounds (Benzothiazole, Benzotriazole, Nitroaniline, Quinoline and some Derivatives) in WastewaterManuscript (preprint) (Other academic)
    Abstract [en]

    Manufacturing of textile consumer goods involve a multitude of chemicals during the entire production chain. In order to investigate the release of harmful compounds from the end products, a sensitive and robust multicomponent procedure for the analysis of three classes of textile related chemicals in aqueous matrices has been developed. The method involves solid phase extraction (SPE) using a graphitized carbon black (GCB) sorbent, followed by GC-MS or LC-MS/MS analysis. The described method can be used to monitor thirty-two selected compounds in waste water. Several of these analytes are regulated by the European Union (REACH) due to their carcinogenic and/or mutagenic properties. After sampling on SPE, three different compound classes are desorbed and analyzed using different chromatographic conditions. The use of GCB provided quantitative and reproducible recoveries of the selected compounds and a cleanup of the wastewater sample. The procedure was evaluated using wastewater sample matrices. Finally, the method was applied in a pilot study to investigate the occurrence of these classes of analytes in the effluent of three different wastewater treatment plants in the Stockholm area. 

  • 4.
    Iadaresta, Francesco
    et al.
    Stockholm University, Faculty of Science, Department of Environmental Science and Analytical Chemistry.
    Crescenzi, Carlo
    Stockholm University, Faculty of Science, Department of Environmental Science and Analytical Chemistry. Universita di Salerno, Italy.
    Amini, Ahmad
    Colmsjö, Anders
    Stockholm University, Faculty of Science, Department of Environmental Science and Analytical Chemistry.
    Koyi, Hirsh
    Abdel-Rehim, Mohamed
    Stockholm University, Faculty of Science, Department of Environmental Science and Analytical Chemistry.
    Application of graphitic sorbent for online microextraction of drugs in human plasma samples2015In: Journal of Chromatography A, ISSN 0021-9673, E-ISSN 1873-3778, Vol. 1422, p. 34-42Article in journal (Refereed)
    Abstract [en]

    In the present work a new sorbent based on graphitized carbon (CarbonX (R) COA) was evaluated in microextraction by packed sorbent (MEPS) for extraction of lidocaine and ropivacaine from human plasma samples. The new graphitic sorbent showed high recoveries of lidocaine and ropivacaine compared to C18 sorbent In the present study the G-MEPS (syringe packed with graphitic sorbent) was connect online with liquid chromatography tandem mass spectrometry (LC-MS/MS). In order to obtain a fast and reliable method different factors affecting MEPS performance were investigated. The extraction efficiency of the graphitic sorbent was compared with silica-based sorbents used in MEPS. The G-MEPS was also evaluated for reuse (50-100 times). The recoveries of lidocaine and ropivacaine from plasma samples were 79% and 82%; respectively. The method was validated according to FDA (Food and Drug Administration) guideline for bioanalytical method validation. Linearity was assessed in the range 5-2000 nmol/L, with coefficient of determination r(2) > 0,995 (n=3) for lidocaine and r(2) > 0.997 (n=3) for ropivacaine. The lower limit of quantification (LLOQ) was 5 nmol/L and the limit of detection (LOD) was 1 nmol/L for studied analytes in plasma samples. For both analytes considered in this study the accuracy values in plasma samples were ranged from 86% to 113%. The Inter-day precisions, expressed as relative standard deviation (%RSD), at three different concentrations (QC-samples) ranged from 8% to 9% for lidocaine, and from 4% to 11% for ropivacaine.

  • 5.
    Iadaresta, Francesco
    et al.
    Stockholm University, Faculty of Science, Department of Environmental Science and Analytical Chemistry.
    Manniello, Michele Dario
    Östman, Conny
    Stockholm University, Faculty of Science, Department of Environmental Science and Analytical Chemistry.
    Crescenzi, Carlo
    Stockholm University, Faculty of Science, Department of Environmental Science and Analytical Chemistry. University of Salerno, Italy.
    Holmbäck, Jan
    Stockholm University, Faculty of Science, Department of Environmental Science and Analytical Chemistry.
    Russo, Paola
    Chemicals from textiles to skin: an in vitro permeation study of benzothiazole2018In: Environmental science and pollution research international, ISSN 0944-1344, E-ISSN 1614-7499, Vol. 25, no 25, p. 24629-24638Article in journal (Refereed)
    Abstract [en]

    Despite the possible impact on human health, few studies have been conducted to assess the penetration and accumulation of contaminants in the skin after a prolonged contact with textile materials. In previous studies, we have shown that benzothiazole and its derivatives, as well as other potentially hazardous chemicals, often are present as textile contaminants in clothes available on the retail market. Since benzothiazole is a common contaminant in clothes, these can be a possible route for human chemical exposure, both systemic and onto the skin. To investigate this potential exposure, Franz-type and flow-through cells were used for the permeation studies together with a Strat-MA (R) artificial membranes. Experiments were performed using solutions of benzothiazole, as well as contaminated textile samples in the donor chamber. Benzothiazole was demonstrated to penetrate through, as well as being accumulated in the membrane mimicking the skin. After 24 h, up to 62% of benzothiazole was found in the acceptor cell, while up to 37% was found absorbed in the skin mimicking membrane. It also was shown that there was release and permeation from contaminated fabrics. The results indicate that benzothiazole can be released from textile materials, penetrate through the skin, and further enter the human body. This will possibly also apply to other chemical contaminants in textiles, and the results of this study indicate that the presence of these textile contaminants entails potential health risks. A rough risk assessment was made for clothing textiles according to Environmental Protection Agency (EPA) and European regulations for carcinogenic and non-carcinogenic compounds, using literature data for benzothiazole.

  • 6.
    Luongo, Giovanna
    et al.
    Stockholm University, Faculty of Science, Department of Environmental Science and Analytical Chemistry.
    Iadaresta, Francesco
    Stockholm University, Faculty of Science, Department of Environmental Science and Analytical Chemistry.
    Moccia, Emanuele
    Crescenzi, Carlo
    Stockholm University, Faculty of Science, Department of Environmental Science and Analytical Chemistry.
    Östman, Conny
    Stockholm University, Faculty of Science, Department of Environmental Science and Analytical Chemistry.
    Aromatic amines in textilesManuscript (preprint) (Other academic)
  • 7.
    Luongo, Giovanna
    et al.
    Stockholm University, Faculty of Science, Department of Environmental Science and Analytical Chemistry.
    Iadaresta, Francesco
    Stockholm University, Faculty of Science, Department of Environmental Science and Analytical Chemistry.
    Moccia, Emanuele
    Stockholm University, Faculty of Science, Department of Environmental Science and Analytical Chemistry.
    Östman, Conny
    Stockholm University, Faculty of Science, Department of Environmental Science and Analytical Chemistry.
    Crescenzi, Carlo
    Stockholm University, Faculty of Science, Department of Environmental Science and Analytical Chemistry. University of Salerno, Italy.
    Determination of aniline and quinoline compounds in textiles2016In: Journal of Chromatography A, ISSN 0021-9673, E-ISSN 1873-3778, Vol. 1471, p. 11-18Article in journal (Refereed)
    Abstract [en]

    A simple method for simultaneous determination of twenty-one analytes, belonging to two classes of compounds, aromatic amines and quinolines, is presented. Several of the analytes considered in this study frequently occur in textiles goods on the open market and have been related to allergic contact dermatitis and/or are proven or suspected carcinogens. The method includes an efficient clean-up step using graphitized carbon black (GCB) that simplifies and improves the robustness of the subsequent GC-MS analysis. Briefly, after solvent extraction of the textile sample, the extract is passed through a GCB SPE cartridge that selectively retain dyes and other interfering compounds present in the matrix, producing a clean extract, suitable for GC-MS analysis, is obtained. The method was evaluated by spiking blank textiles with the selected analytes. Method quantification limits (MQL) ranged from 5 to 720 ng/g depending on the analyte. The linear range of the calibration curves ranged over two order magnitude with coefficients of determination (R-2) higher than 0.99. Recoveries ranged from 70 to 92% with RSDs 1.7-14%. The effectiveness of the method was tested on a variety of textile materials samples from different origin. In a pilot explorative survey, 2,6-dichloro-4-nitroaniline was detected in all the analysed clothing samples in concentrations ranging from 1.0 to 576 mu g/g 2,4-dinitroaniline was detected in four of the seven samples with a highest concentration of 305 mu g/g Quinoline was detected in all samples in concentrations ranging from 0.06 to 6.2 mu g/g. (C) 2016 Elsevier B.V. All rights reserved.

  • 8.
    Shariatgorji, Mohammadreza
    et al.
    Stockholm University, Faculty of Science, Department of Analytical Chemistry.
    Amini, Nahid
    Stockholm University, Faculty of Science, Department of Analytical Chemistry.
    Thorsen, Gunnar
    Stockholm University, Faculty of Science, Department of Analytical Chemistry.
    Crescenzi, Carlo
    Stockholm University, Faculty of Science, Department of Analytical Chemistry.
    Ilag, Leopold
    Stockholm University, Faculty of Science, Department of Analytical Chemistry.
    µ-trap for the SALDI-MS screening of organic compounds prior to LC/MS analysis2008In: Analytical Chemistry, ISSN 0003-2700, E-ISSN 1520-6882, Vol. 80, no 14, p. 5515-5523Article in journal (Refereed)
    Abstract [en]

    A procedure for rapidly screening and quantitatively analyzing organic molecules is presented, in which a miniaturized solid-phase extraction (SPE) cartridge containing 0.6 mg of graphitized carbon black (the GCB-mu-trap) is used for sample pretreatment. Then surface-assisted laser desorption ionization dine-of-flight mass spectrometry (SALDI-TOF-MS) screening is followed by liquid chromatography/mass spectrometry (LC/MS) for robust quantitative analysis of samples containing analytes of interest. Liquid samples with volumes up to 100 mL were extracted using the GCB-mu-trap, and SALDI screening was performed by transferring a few particles of the GCB 4 sorbent from the mu-trap onto a stainless steel plate. Analytes were then simply ionized and desorbed by irradiating the GCB 4 particles without any further pretreatment. GCB 4 was found to be an excellent surface for the SALDI analysis of small molecules, providing spectra with very clean backgrounds. The small size of the cartridge (micropipet filter tip) results in enrichment of the analytes on a small surface area, affording low SALDI-TOF-MS detection limits. Furthermore, the removal of just a few particles from the p-trap does not significantly affect the subsequent quantitative determination. This approach offers considerable reductions in analytical costs by eliminating unnecessary SPE-LC/MS analyses.

  • 9.
    Tollbäck, J
    et al.
    Stockholm University, Faculty of Science, Department of Analytical Chemistry.
    Bigata, M B
    Crescenzi, C
    Stockholm University, Faculty of Science, Department of Analytical Chemistry.
    Strom, J
    Feasibility of Analyzing Fine Particulate Matter in Air Using Solid-Phase Extraction Membranes and Dynamic Subcritical Water Extraction2008In: Analytical Chemistry, Vol. 80, p. 3159-3167Article in journal (Refereed)
  • 10.
    Tollbäck, Johanna
    et al.
    Stockholm University, Faculty of Science, Department of Analytical Chemistry.
    Bigatá, María Blasco
    Crescenzi, Carlo
    Stockholm University, Faculty of Science, Department of Analytical Chemistry.
    Ström, Johan
    Stockholm University, Faculty of Science, Department of Applied Environmental Science (ITM).
    Feasibility of analyzing fine particulate matter in air using solid-phase extraction membranes and dynamic subcritical water extraction2008In: Analytical chemistry, ISSN 1520-6882, Vol. 80, no 9, p. 3159-67Article in journal (Refereed)
    Abstract [en]

    We have evaluated the feasibility of using Empore solid-phase extraction (SPE) membranes as an alternative to conventional techniques for sampling fine airborne particulate matter (PM), including nanoparticles, utilizing a scanning mobility particle sizer (SMPS) and a condensation particle counter to evaluate their efficiency for trapping fine particles in the 10-800 nm size range. The results demonstrate that the membranes can efficiently trap these particles and can then be conveniently packed into an extraction cell and extracted under matrix solid-phase dispersion (MSPD) conditions. The potential utility of sampling PM using Empore membranes followed by dynamic subcritical water extraction (DSWE) for fast, efficient, class-selective extraction of polycyclic aromatic hydrocarbons (PAHs) associated with the particles, prior to changing the solvent and analysis by GC/MS, was then explored. The performance of the method was tested using National Institute of Standards and Technology (NIST)-certified "urban dust" reference material (SRM 1649a) and real samples collected at a site in central Rome with heavy road traffic. The method appears to provide comparable extraction efficiency to that of conventional techniques and with using GC/MS, detection limits ranged in the few picograms per cubic meter level. Sampling PM by Empore membranes may reduce the risks of losses of semivolatile compounds, while allowing relatively high sampling flow rates and safe sample storage. Moreover, the combination of MSPD with DSWE permits specific fractions of the PM components to be eluted, thereby generating clean extracts and reducing both analysis time and sample manipulation.

  • 11.
    Tollbäck, Johanna
    et al.
    Stockholm University, Faculty of Science, Department of Analytical Chemistry.
    Crescenzi, Carlo
    Stockholm University, Faculty of Science, Department of Analytical Chemistry.
    Dyremark, Eva
    Determination of the flame retardant tetrabromobisphenol A in air samples by liquid chromatography-mass spectrometry.2006In: Journal of Chromatography A, ISSN 0021-9673, E-ISSN 1873-3778, Vol. 1104, no 1-2, p. 106-12Article in journal (Refereed)
    Abstract [en]

    An original method based on LC-MS for determination of the flame retardant tetrabromobisphenol A (TBBPA) in air is presented, as an alternative to the traditionally used GC-MS. The soft ionization in LC-MS makes it possible to monitor the intact molecule and to use 13C-labelled TBBPA as an internal surrogate standard, two features that improve both accuracy and precision of the analyses. Comparison of different acquisition modes in electrospray ionization showed that the lowest detections limit, 3.1 pg TBBPA injected, was obtained in SIM monitoring the molecular ions 542.7/544.7. A fragmentation pathway of TBBPA in LC-ESI-MS is suggested. The only sample clean-up steps required are solvent reduction and filtration of the sample extract. Recoveries were 93% at a 30 ng level and 75% at 3 ng. The new method was tested by analyses of air samples collected at a recycling plant for electronic equipment. The amount of TBBPA found was 13.8 ng/m3 with an RSD of 5.9%. Furthermore, it was found that TBBPA in a standard solution could be partially debrominated, if not carefully protected from light during storage.

  • 12.
    Tollbäck, Johanna
    et al.
    Stockholm University, Faculty of Science, Department of Analytical Chemistry.
    Tamburro, Davide
    Stockholm University, Faculty of Science, Department of Analytical Chemistry.
    Crescenzi, Carlo
    Stockholm University, Faculty of Science, Department of Analytical Chemistry.
    Carlsson, Håkan
    Stockholm University, Faculty of Science, Department of Analytical Chemistry.
    Air sampling with Empore solid phase extraction membranes and online single-channel desorption/liquid chromatography/mass spectrometry analysis: Determination of volatile and semi-volatile organophosphate esters2006In: Journal of Chromatography A, ISSN 0021-9673, E-ISSN 1873-3778, Vol. 1129, no 1, p. 1-8Article in journal (Refereed)
    Abstract [en]

    A method for determining organophosphate esters in air samples using C8 Empore solid phase extraction (SPE) membranes has been developed. After the sampling the analytes trapped in the membrane are completely desorbed with methanol, using an extraction cell connected online to the organic modifier channel of a HPLC gradient pump. The addition of water to the mobile phase prior to analytical chromatography ensures that the analytes are refocused and efficiently separated. Sampling with Empore SPE membranes enables the collection of analytes in both the vapour phase and particulate matter. During the air sampling procedure no losses were observed after 24 h of sampling, yielding a total volume of 14.4 m3, even for the most volatile compound used in this investigation (trimethylphosphate). Complete desorption was observed for all the organophosphate esters and recoveries were greater than 95%, with a relative standard deviation of less than 8%. The limits of detection ranged between 0.4 and 19 pg/m3. The effect of particulate matter on the extraction efficiency was investigated in detail by spiking the membranes with reference standard material. It was also found that the SPE membranes could be stored for at least 5 days at room temperature without any evidence of loss. The efficacy of the method was verified using real samples from different common indoor environments. Interestingly, significant quantities of several phosphate esters were found in a NIST standard reference material (urban dust, SRM 1649a).

  • 13.
    Wincent, Emma
    et al.
    Stockholm University, Faculty of Science, Department of Genetics, Microbiology and Toxicology.
    Amini, Nahid
    Stockholm University, Faculty of Science, Department of Analytical Chemistry.
    Luecke, Sandra
    Glatt, H.
    Bergman, Jan
    Crescenzi, Carlo
    Stockholm University, Faculty of Science, Department of Analytical Chemistry.
    Rannug, Agneta
    Rannug, Ulf
    Stockholm University, Faculty of Science, Department of Genetics, Microbiology and Toxicology.
    The suggested physiologic aryl hydrocarbon receptor activator and cytochrome P4501 substrate 6-formylindolo[3,2-b]carbazole is present in humans2009In: Journal of Biological Chemistry, ISSN 0021-9258, E-ISSN 1083-351X, Vol. 284, no 5, p. 2690-2696Article in journal (Refereed)
    Abstract [en]

    Dioxins and other polycyclic aromatic compounds formed during the combustion of waste and fossil fuels represent a risk to human health, as well as to the well being of our environment. Compounds of this nature exert carcinogenic and endocrine-disrupting effects in experimental animals by binding to the orphan aryl hydrocarbon receptor (AhR). Understanding the mechanism of action of these pollutants, as well as the physiological role(s) of the AhR, requires identification of the endogenous ligand(s) of this receptor. We reported earlier that activation of AhR by ultraviolet radiation is mediated by the chromophoric amino acid tryptophan (Trp), and we suggested that a new class of compounds derived from Trp, in particular 6-formylindolo[3,2-b]carbazole (FICZ), acts as natural high affinity ligands for this receptor. Here we describe seven new FICZ-derived indolo[3,2-b]carbazole-6-carboxylic acid metabolites and two sulfoconjugates, and we demonstrate the following. (i) FICZ is formed efficiently by photolysis of Trp upon exposure to visible light. (ii) FICZ is an exceptionally good substrate for cytochromes P450 (CYP) 1A1, 1A2, and 1B1, and its hydroxylated metabolites are remarkably good substrates for the sulfotransferases (SULTs) 1A1, 1A2, 1B1, and 1E1. Finally, (iii) sulfoconjugates of phenolic metabolites of FICZ are present in human urine. Our findings indicate that formylindolo[3,2-b]carbazols are the most potent naturally occurring activators of the AhR signaling pathway and may be the key substrates of the CYP1 and SULT1 families of enzymes. These conclusions contradict the widespread view that xenobiotic compounds are the major AhR ligands and CYP1 substrates.

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