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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
Stockholm University, Faculty of Science, Department of Analytical Chemistry.
Stockholm University, Faculty of Science, Department of Analytical Chemistry.
Stockholm University, Faculty of Science, Department of Analytical Chemistry.
Stockholm University, Faculty of Science, Department of Analytical Chemistry.
2006 (English)In: Journal of Chromatography A, ISSN 0021-9673, E-ISSN 1873-3778, Vol. 1129, no 1, 1-8 p.Article in journal (Refereed) Published
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).

Place, publisher, year, edition, pages
2006. Vol. 1129, no 1, 1-8 p.
Keyword [en]
Air sampling; Air analysis; Online; Single-channel desorption; Dynamic solvent extraction; Extraction methods; LC-MS; Volatile; Semi-volatile; Organophosphate esters; Empore disk; Solid phase extraction; SPE; Membranes; Particulate matter; Urban dust; Environmental analysis; Organophosphorus compounds; Phosphate
National Category
Analytical Chemistry
Research subject
Analytical Chemistry
Identifiers
URN: urn:nbn:se:su:diva-26595DOI: 10.1016/j.chroma.2006.05.086PubMedID: 16934277OAI: oai:DiVA.org:su-26595DiVA: diva2:211074
Available from: 2009-04-07 Created: 2009-04-02 Last updated: 2017-12-13Bibliographically approved
In thesis
1. New methods for determination of airborne pollutants: Focus on tetrabromobisphenol A, organophosphate triesters and polycyclic aromatic hydrocarbons
Open this publication in new window or tab >>New methods for determination of airborne pollutants: Focus on tetrabromobisphenol A, organophosphate triesters and polycyclic aromatic hydrocarbons
2009 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

The work presented in this thesis concerns the development and evaluation of new methods of sampling and analysis of organic pollutants in the indoor and outdoor environment.

In Paper I, the development of a new method was reported for the determination of the brominated flame retardant tetrabromobisphenol A (TBBPA) in air using sampling with glass fiber filter and polyurethane foam (PUF), ultrasonic solvent extraction and liquid chromatography coupled to electrospray ionisation mass spectrometry (LC-ESI/MS). The MS fragmentation mechanism of TBBPA was thoroughly investigated and different acquisition modes were evaluated to achieve the most sensitive and selective detection.

In Papers II and III, the potential use of Empore SPE membranes was evaluated for air sampling of volatile, semi-volatile and particle-associated organic compounds. Breakthrough studies conducted for 24h at air flows of 10- 20 L/min showed that the SPE membranes efficiently retains volatile and semi-volatile organophosphate esters and particles >10 nm. Effort was invested in the development of fast and environmental friendly methods, with low cost, for sample clean up and analysis.

In Paper II, the sample preparation technique was dynamic solvent extraction with methanol coupled to LC-ESI/MS. The total run time per sample, including both extraction and separation, was less than 34 min, consuming only 1.6mL methanol. In Paper III, efficiency of selective extraction of polycyclic aromatic hydrocarbons from particulate matter sampled with Empore SPE membranes, using dynamic subcritical water extraction (DSWE) was investigated. Acceptable recoveries of the investigated compounds from reference material (SRM 1649a) were achieved. In Paper IV, the application of dynamic solid phase micro-extraction (SPME) air sampling was evaluated using, gas chromatography/positive ion chemical ionisation (GC/PICI) and tandem-MS detection for the determination of organophosphate esters in work environment.

Place, publisher, year, edition, pages
Stockholm: Department of Analytical Chemistry, Stockholm University, 2009. 80 p.
Keyword
Air sampling, sampling methods, indoor air, SPE, SPME, extraction, dynamic extraction, online coupling, SWE, subcritical water extraction, GC/MS, LC/MS, organophosphate triesters, PAH, tetrabromobisphenol A
National Category
Analytical Chemistry
Research subject
Analytical Chemistry
Identifiers
urn:nbn:se:su:diva-26700 (URN)978-91-7155-843-5 (ISBN)
Public defence
2009-05-14, Magnélisalen, Kemiska Övningslaboratoriet, Svante Arrhenius väg 12 A, Stockholm, 13:00 (Swedish)
Opponent
Supervisors
Available from: 2009-04-23 Created: 2009-04-07 Last updated: 2010-12-14Bibliographically approved
2. Colloidal/Solid Phase Extraction (C/S PE) Methods Based on Hydrogel Nanoparticles, Titanium dioxide microparticles and Empore Membranes Applied to Biological and Environmental Matrices
Open this publication in new window or tab >>Colloidal/Solid Phase Extraction (C/S PE) Methods Based on Hydrogel Nanoparticles, Titanium dioxide microparticles and Empore Membranes Applied to Biological and Environmental Matrices
2011 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

The aim of the work described in this thesis was to create and develop novel technologies in order to overcome barriers and hurdles that analytical chemistry faces focusing on sample extraction. In paper I dye containing amine groups (e.g. Acid Black 48, Remazol Brilliant Blue R) were coupled to NIPA/Acrylic acid (AAc) particles by condensation of the amine group and the carboxylic group. The high affinity between dyes and proteins allow for fast kinetics and complete depletion of the supernatant and protection of the captured analyte from enzymatic degradation. The ability of particles to capture and concentrate analytes was tested against a panel of low abundance, labile tumor relevant biomarkers and in serum. Results indicate that the nanoparticles increased the sensitivity limit of mass spectrometry analysis and that the dye based baits have extremely high affinity for the target analytes so that particles capture all the analyte present in solution. Biomarker harvesting nanoparticles may be useful for discovery of novel diagnostic analytes, can increase the sensitivity of detection for analytical methods such as immunoassays and MS, and protect labile biomarkers from degradation during collection, shipment and storage. In paper II and paper III, applications of hydrogel nanoparticles to serum samples from cancer patients are reported. Hydrogel nanoparticles were integrated in a mass spectrometry based workflow for the discovery of candidate biomarkers. Lists of candidate biomarkers were identified that are under verification and validation. In paper IV and V hydrogel nanoparticles functionalized with dyes, were employed to increase the sensitivity of diagnostic test for Lyme disease and to detect human growth hormone (hGH) in urine samples. In paper VI, titanium dioxide (TiO2) microparticles were used to pack fused silica capillary column and used to capture and enrich phosphopeptides in vitreous samples. In paper VII, Empore disk membranes were used to capture organophosphates (OPEs) flame retardant from air samples. Empore disk membranes were used as on- line extraction followed by reverse phase liquid chromatography tandem mass spectrometry (RPLC-MS/MS) analysis. Optimized “geometry” settings were used to strip semi volatile and volatile compounds from C8 membrane. This novel design allowed for a better analyte focusing in the HPLC column, reduced the volume of the organic solvent employed for the extraction and the analysis time, and eliminated sample contamination, and loss of analyte.

Place, publisher, year, edition, pages
Stockholm: Department of Analytical Chemistry, Stockholms University, 2011. 110 p.
Keyword
biomarkers, nanogels, solid-phase extraction, organophosphate esters, peptides, mass spectrometry
National Category
Analytical Chemistry
Research subject
Analytical Chemistry
Identifiers
urn:nbn:se:su:diva-56873 (URN)978-91-7447-231-8 (ISBN)
Public defence
2011-06-01, Magnélisalen, Kemiska övningslaboratoriet, Svante Arrhenius väg 16 B, Stockholm, 13:00 (English)
Opponent
Supervisors
Note
At the time of the doctoral defense, the following papers were unpublished and had a status as follows: Paper 5: Manuscript. Paper 6: Manuscript.Available from: 2011-05-10 Created: 2011-04-28 Last updated: 2011-05-02Bibliographically approved

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