Determination of volatile organic compounds in water by headspace solid-phase microextraction gas chromatography coupled to tandem mass spectrometry with triple quadrupole analyzer

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• 作者：M.I.  ; Cervera ; J.  ; Beltran  ; ;   ; ^{joaquim.beltran@uji.es} ; F.J.  ; Lopez ; F.  ; Hernandez
• 关键词：Volatile organic compounds ; Gas chromatography tandem mass spectrometry ; Triple quadrupole ; Environmental water ; Wastewater ; Headspace solid-phase microextraction
• 刊名：Analytica Chimica Acta
• 出版年：2011
• 出版时间：17 October 2011
• 年：2011
• 卷：704
• 期：1-2
• 页码：87-97
• 全文大小：1679 K

文摘

In the present work, a rapid method with little sample handling has been developed for determination of 23 selected volatile organic compounds in environmental and wastewater samples. The method is based on headspace solid-phase microextraction (SPME) followed by gas chromatography coupled to tandem mass spectrometry (GC¨CMS/MS) determination using triple quadrupole analyzer (QqQ) in electron ionization mode. The best conditions for extraction were optimised with a factorial design taking into account the interaction between different parameters and not only individual effects of variables. In the optimized procedure, 4 mL of water sample were extracted using a 10 mL vial and adding 0.4 g NaCl (final NaCl content of 10 % ). An SPME extraction with carboxen/polydimethylsiloxane 75 ¦Ìm fiber for 30 min at 50 ¡ãC (with 5 min of previous equilibration time) with magnetic stirring was applied. Chromatographic determination was carried out by GC¨CMS/MS working in Selected Reaction Monitoring (SRM) mode. For most analytes, two MS/MS transitions were acquired, although for a few compounds it was difficult to obtain characteristic abundant fragments. In those cases, a pseudo selected reaction monitoring (pseudo-SRM) with three ions was used instead. The intensity ratio between quantitation (Q) and confirmation (q) signals was used as a confirmatory parameter.

The method was validated by means of recovery experiments (n = 6) spiking mineral water samples at three concentration levels (0.1, 5 and 50 ¦Ìg L^?). Recoveries between 70 % and 120 % were generally obtained with relative standard deviations (RSDs) lower than 20 % .

The developed method was applied to surface water and wastewater from a wastewater treatment plant and from a municipal solid-waste treatment plant. Several compounds, like chloroform, benzene, trichloroethylene, toluene, tetrachloroethylene, dibromochloromethane, xylenes and bromoform were detected and confirmed in all the samples analyzed.