| 1. |
- Amini, Nahid, et al.
(författare)
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Feasibility of an on-line restricted access material/liquidchromatography/tandem mass spectrometry method in the rapid and sensitive determination of organophosphorustriesters in human blood plasma
- 2003
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Ingår i: Journal of chromatography. B. - 1570-0232 .- 1873-376X. ; 795:2, s. 245-256
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Tidskriftsartikel (refereegranskat)abstract
- A rapid on-line solid phase extraction/liquid chromatography/tandem mass spectrometry (SPE/LC/MS/MS) method usingrestricted access material (RAM) was developed for the simultaneous determination of eight organophosphorus triesters inuntreated human blood plasma. In a process involving column-switching techniques, the analytes were enriched on the RAMcolumn, separated using a C-18 analytical column and detected with LC/MS. Tandem mass spectrometrywas used to characterizeand quantify the analytes. To elucidate the fragmentation pathway of a number of the analytes, MS3 experiments using an iontrap mass spectrometer were performed. The matrix effects associated with using APCI and ESI interfaces were investigated.The recoveries obtained were in the range 60–92% (R.S.D. < 6%), with estimated detection limits between 0.2 and 1.8 ng/mlof plasma, and the total analysis time was 27 min.
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| 2. |
- Amini, Nahid, et al.
(författare)
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Screening and Quantification of Pesticides in Water Using a Dual-Function Graphitized Carbon Black Disk
- 2010
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Ingår i: Analytical Chemistry. - : ACS. - 0003-2700 .- 1520-6882. ; 82:1, s. 290-296
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Tidskriftsartikel (refereegranskat)abstract
- A simple platform for combining solid phase extraction (SPE) and surface-assisted laser desorption ionization mass spectrometry (SALDI-MS) of extracted analytes, using disks prepared by embedding graphitized carbon black (GCB-4) particles in a network of polytetrafluoroethylene (PTFE), is presented. The system provides a convenient approach for rapid SALDI-MS screening of substances in aqueous samples, which can be followed by robust quantitative and/or structural analyses by liquid chromatography (LC)/MS/MS of positive samples. The extraction discs are easily transferred between gaskets where the sample extraction and desorption of selected samples is performed and the mass spectrometer. The SPE and SALDI properties of the new GCB-4 disc have been characterized for 15 pesticides with varying chemical properties, and the screening strategy has been applied to the analysis of pesticides in agricultural drainage water. Atrazine and atrazine-desethyl-2-hydroxy were detected in the sampled water by SALDI-MS screening and subsequently confirmed and quantified using LC/MS/MS.
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| 3. |
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| 4. |
- Grasso, Giuliana, et al.
(författare)
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Enhanced selective capture of phosphomonoester lipids enabling highly sensitive detection of sphingosine 1-phosphate
- 2023
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Ingår i: Analytical and Bioanalytical Chemistry. - : Springer. - 1618-2642 .- 1618-2650. ; 415:26, s. 6573-6582
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Tidskriftsartikel (refereegranskat)abstract
- Sphingolipids play crucial roles in cellular membranes, myelin stability, and signalling responses to physiological cues and stress. Among them, sphingosine 1-phosphate (S1P) has been recognized as a relevant biomarker for neurodegenerative diseases, and its analogue FTY-720 has been approved by the FDA for the treatment of relapsing-remitting multiple sclerosis. Focusing on these targets, we here report three novel polymeric capture phases for the selective extraction of the natural biomarker and its analogue drug. To enhance analytical performance, we employed different synthetic approaches using a cationic monomer and a hydrophobic copolymer of styrene-DVB. Results have demonstrated high affinity of the sorbents towards S1P and fingolimod phosphate (FTY-720-P, FP). This evidence proved that lipids containing phosphate diester moiety in their structures did not constitute obstacles for the interaction of phosphate monoester lipids when loaded into an SPE cartridge. Our suggested approach offers a valuable tool for developing efficient analytical procedures.
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| 5. |
- Iadaresta, Francesco, et al.
(författare)
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Application of graphitic sorbent for online microextraction of drugs in human plasma samples
- 2015
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Ingår i: Journal of Chromatography A. - : Elsevier BV. - 0021-9673 .- 1873-3778. ; 1422, s. 34-42
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Tidskriftsartikel (refereegranskat)abstract
- 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.
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| 6. |
- Iadaresta, Francesco, et al.
(författare)
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Chemicals from textiles to skin : an in vitro permeation study of benzothiazole
- 2018
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Ingår i: Environmental Science and Pollution Research. - : Springer Science and Business Media LLC. - 0944-1344 .- 1614-7499. ; 25:25, s. 24629-24638
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Tidskriftsartikel (refereegranskat)abstract
- 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.
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| 7. |
- Iadaresta, Francesco, 1985-, et al.
(författare)
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Determination of Textile Related Compounds (Benzothiazole, Benzotriazole, Nitroaniline, Quinoline and some Derivatives) in Wastewater
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Annan publikation (övrigt vetenskapligt/konstnärligt)abstract
- 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.
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| 8. |
- Iadaresta, Francesco, 1985-
(författare)
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Textile Related Chemicals: Analytical Approaches Towards the Assessment of Human and Environmental Exposures
- 2019
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Doktorsavhandling (övrigt vetenskapligt/konstnärligt)abstract
- The textile manufacturing chain involves an extensive use of chemicals as early as fabric-production. To confer special features to textile materials, more chemicals are required in subsequent steps. Furthermore, potentially harmful substances can end up in clothes as transformation products. Compounds that are not covalently bonded to the fabrics have high probability to be released on the skin or into the environment when the clothes are worn or laundered.In order to remove interfering compounds from solvent extracts of investigated textiles, a cleanup step based on solid phase extraction using graphitic carbon black was developed resulting in effective dye removal. In a pilot screening, nitroanilines were detected up to 0.57 mg/g, which was 2-3 order of magnitude higher than measured quinolines.Human exposure to chemicals can occur through skin contact. Benzothiazole was chosen as model compound for in-vitro experiments. Its permeation was experimentally determined in order to estimate dermal exposure. Carcinogenic and non-carcinogenic risks, associated to wearing t-shirt containing BT, according to international standards, were found to be below the acceptable exposure levels.It has been shown that chemical concentrations decreased during domestic washing. A procedure was developed for enrichment and clean-up of textile related compounds from water samples. The method was applied to three wastewater treatment plant effluents located in Stockholm. Tolyltriazole, 1-benzotriazole, and UV-P were detected within the range of 53-1148 ng/L.Suspect and non-target screening methodology was developed do detect and identify substances in textile materials. The occurrence of thirteen suspect compounds, belonging to quinolines, nitroanilines, benzotriazoles, benzothiazoles and phthalates, was confirmed through suspect analysis approach. Furthermore, using a non-target screening approach, compounds not included in the suspect list such as nitrophenols, organophosphate and acridine were identified.In order to remove interfering compounds from the textile extracts, a cleanup step based on solid phase extraction using graphitic carbon black was developed resulting in effective dye removal. In a pilot screening, nitroanilines were detected up to 0.57 mg/g, which was 2-3 times higher than measured quinolines.Human exposure to chemicals can occur through skin contact. Benzothiazole was chosen as model compound for in-vitro experiments. Its permeation was experimentally determined in order to estimate dermal exposure. Carcinogenic and non-carcinogenic risks, associated to wearing t-shirt containing BT, according to international standards, were found to be below the acceptable exposure levels.It has been shown that chemical concentrations decreased during domestic washing. A procedure was developed for enrichment and clean-up of textile related compounds from water samples. The method was applied to three wastewater treatment plant effluents located in Stockholm. Tolyltriazole, 1-benzotriazole, and UV-P were detected within the range of 53-1148 ng/L. Suspect and non-target screening methodology was developed do detect and identify substances in textile materials. The occurrence of thirteen suspect compounds, belonging to quinolines, nitroanilines, benzotriazoles, benzothiazoles and phthalates, was confirmed through suspect approach. Furthermore, using a non-target screening approach, compounds not included in suspect list such as nitrophenols, organophosphate and acridine were identified.
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| 9. |
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| 10. |
- Luongo, Giovanna, et al.
(författare)
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Determination of aniline and quinoline compounds in textiles
- 2016
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Ingår i: Journal of Chromatography A. - : Elsevier BV. - 0021-9673 .- 1873-3778. ; 1471, s. 11-18
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Tidskriftsartikel (refereegranskat)abstract
- 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.
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| 11. |
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| 12. |
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| 13. |
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| 14. |
- Shariatgorji, Mohammadreza, 1974-, et al.
(författare)
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µ-trap for the SALDI-MS screening of organic compounds prior to LC/MS analysis
- 2008
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Ingår i: Analytical Chemistry. - : ACS. - 0003-2700 .- 1520-6882. ; 80:14, s. 5515-5523
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Tidskriftsartikel (refereegranskat)abstract
- 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.
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| 15. |
- Tollbäck, Johanna, et al.
(författare)
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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 esters
- 2006
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Ingår i: Journal of Chromatography A. - : Elsevier BV. - 0021-9673 .- 1873-3778. ; 1129:1, s. 1-8
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Tidskriftsartikel (refereegranskat)abstract
- 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).
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| 16. |
- Tollbäck, Johanna, et al.
(författare)
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Determination of the flame retardant tetrabromobisphenol A in air samples by liquid chromatography-mass spectrometry.
- 2006
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Ingår i: Journal of Chromatography A. - : Elsevier BV. - 0021-9673 .- 1873-3778. ; 1104:1-2, s. 106-12
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Tidskriftsartikel (refereegranskat)abstract
- 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.
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| 17. |
- Tollbäck, Johanna, et al.
(författare)
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Feasibility of analyzing fine particulate matter in air using solid-phase extraction membranes and dynamic subcritical water extraction
- 2008
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Ingår i: Analytical chemistry. - : American Chemical Society (ACS). - 1520-6882 .- 0003-2700. ; 80:9, s. 3159-67
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Tidskriftsartikel (refereegranskat)abstract
- 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.
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| 18. |
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| 19. |
- Wincent, Emma, et al.
(författare)
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The suggested physiologic aryl hydrocarbon receptor activator and cytochrome P4501 substrate 6-formylindolo[3,2-b]carbazole is present in humans
- 2009
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Ingår i: Journal of Biological Chemistry. - 0021-9258 .- 1083-351X. ; 284:5, s. 2690-2696
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Tidskriftsartikel (refereegranskat)abstract
- 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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