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J Chromatogr A


Title:Analysis of 35 priority semivolatile compounds in water by stir bar sorptive extraction-thermal desorption-gas chromatography-mass spectrometry. I. Method optimisation
Author(s):Leon VM; Alvarez B; Cobollo MA; Munoz S; Valor I;
Address:"Labaqua S.A., C/Alona 33, 03007 Alicante, Spain"
Journal Title:J Chromatogr A
Year:2003
Volume:999
Issue:1-Feb
Page Number:91 - 101
DOI: 10.1016/s0021-9673(03)00600-9
ISSN/ISBN:0021-9673 (Print) 0021-9673 (Linking)
Abstract:"A multiresidue method for the determination of 35 organic micropollutants (pesticides and polycyclic aromatic hydrocarbons) in water has been optimised using stir bar sorptive extraction (SBSE) and thermal desorption coupled to capillary gas chromatography-mass spectrometry (GC-MS). In the present work, the different parameters affecting the extraction of the analytes from the water samples to the PDMS-coated stir bars and optimisation of conditions affecting thermal desorption are investigated. The optimised conditions consist of a 100-ml water sample with 20% NaCl addition extracted with 20 mm length x 0.5 mm film thickness stir bars at 900 rpm during 14 h at ambient temperature. Desorption is carried out at 280 degrees C during 6 min under a helium flow of 75 ml/min in the splitless mode while maintaining a cryofocusing temperature of 20 degrees C in the programmed-temperature vaporisation (PTV) injector of the GC-MS system. Finally, the PTV injector is ramped to a temperature of 280 degrees C and the analytes are separated in the GC and detected by MS using full scan mode (m/z 60-400). Under the described conditions, the good repeatability, high analyte recoveries and robustness, make SBSE a powerful tool for routine quality control analysis of the selected semivolatile compounds in water samples"
Keywords:Adsorption Gas Chromatography-Mass Spectrometry/*methods Volatilization Water/*chemistry;
Notes:"MedlineLeon, V M Alvarez, B Cobollo, M A Munoz, S Valor, I eng Netherlands 2003/07/30 J Chromatogr A. 2003 May 30; 999(1-2):91-101. doi: 10.1016/s0021-9673(03)00600-9"

 
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