PMID- 18456273
OWN - NLM
STAT- MEDLINE
DCOM- 20080924
LR  - 20090115
IS  - 0021-9673 (Print)
IS  - 0021-9673 (Linking)
VI  - 1196-1197
DP  - 2008 Jul 4
TI  - Determination of basic degradation products of chemical warfare agents in water 
      using hollow fibre-protected liquid-phase microextraction with in-situ 
      derivatisation followed by gas chromatography-mass spectrometry.
PG  - 125-32
LID - 10.1016/j.chroma.2008.04.027 [doi]
AB  - Hollow fibre-protected liquid-phase microextraction (HF-LPME) together with gas 
      chromatography-mass spectrometry was, for the first time, investigated for the 
      in-situ derivatisation and analysis of basic degradation products of chemical 
      warfare agents in water samples. The degradation products studied were those of 
      nerve and blister agents, and a psychotomimetic agent. Extractions with in-situ 
      derivatisation were successfully performed using a mixture of solvent and 
      derivatising agent. The protection of the moisture-sensitive derivatising agent 
      was afforded by the hydrophobic hollow fibre. Parameters such as type of 
      derivatising agent, extraction solvent, pH, salt concentration, stirring speed 
      and extraction time were optimised using spiked deionised water samples. The 
      linear range established was between 0.05 and 25 microg ml(-1) depending on 
      analyte, with squared regression coefficients ranging from 0.9959 to 0.9996. 
      Relative standard deviations (RSDs) ranged from 6% to 10%. As comparison, 
      solid-phase microextraction (SPME) was also evaluated and extraction conditions 
      such as pH, salt concentration, stirring speed and extraction time were 
      optimised. This work also represented the first report of such an in-situ 
      derivatisation approach for SPME of basic analytes. The linear range established 
      was between 0.5 and 25 microg ml(-1) depending on analyte, with squared 
      regression coefficients ranging from 0.9946 to 0.9998. RSDs ranged from 5% to 
      22%. The limits of detection of HF-LPME (0.04-0.36 microg l(-1)) showed 
      improvement over those of SPME (0.06-0.77 microg l(-1)).
FAU - Lee, Hoi Sim Nancy
AU  - Lee HS
AD  - DSO National Laboratories, 20 Science Park Drive, Singapore, Singapore.
FAU - Sng, Mui Tiang
AU  - Sng MT
FAU - Basheer, Chanbasha
AU  - Basheer C
FAU - Lee, Hian Kee
AU  - Lee HK
LA  - eng
PT  - Journal Article
PT  - Research Support, Non-U.S. Gov't
DEP - 20080420
PL  - Netherlands
TA  - J Chromatogr A
JT  - Journal of chromatography. A
JID - 9318488
RN  - 0 (Chemical Warfare Agents)
SB  - IM
MH  - Chemical Fractionation/*methods
MH  - Chemical Warfare Agents/*analysis/chemistry
MH  - Gas Chromatography-Mass Spectrometry/*methods
MH  - Molecular Structure
MH  - Reproducibility of Results
EDAT- 2008/05/06 09:00
MHDA- 2008/09/25 09:00
CRDT- 2008/05/06 09:00
PHST- 2008/02/16 00:00 [received]
PHST- 2008/04/11 00:00 [revised]
PHST- 2008/04/15 00:00 [accepted]
PHST- 2008/05/06 09:00 [pubmed]
PHST- 2008/09/25 09:00 [medline]
PHST- 2008/05/06 09:00 [entrez]
AID - S0021-9673(08)00705-X [pii]
AID - 10.1016/j.chroma.2008.04.027 [doi]
PST - ppublish
SO  - J Chromatogr A. 2008 Jul 4;1196-1197:125-32. doi: 10.1016/j.chroma.2008.04.027. 
      Epub 2008 Apr 20.