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Speciation of volatile antimony compounds in culture headspace gases of Cryptococcus humicolus using solid phase microextraction and gas chromatography–mass spectrometry
Author(s) -
Smith L. M.,
Maher W. A.,
Craig P. J.,
Jenkins R. O.
Publication year - 2002
Publication title -
applied organometallic chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.53
H-Index - 71
eISSN - 1099-0739
pISSN - 0268-2605
DOI - 10.1002/aoc.303
Subject(s) - antimony , chemistry , stibine , chromatography , mass spectrometry , solid phase microextraction , gas chromatography , gas chromatography–mass spectrometry , extraction (chemistry) , analytical chemistry (journal) , inorganic chemistry , organic chemistry , arsine , phosphine , catalysis
Direct analysis of the volatile antimony compounds stibine (SbH 3 ), monomethylantimony, dimethylantimony (Me 2 Sb) and trimethylantimony (Me 3 Sb) using solid phase microextraction (SPME) with polydimethylsiloxane fibres and gas chromatography–mass spectrometry (GC–MS) is described. The best analyte to background signal ratio was achieved using a 20 min extraction time. Antimony species were separated using a 3% phenylmethylsilicone capillary column operated at a column pressure of 70 kPa, a flow rate of 1.4 ml min −1 and temperature ramping from 30 to 36 °C at 0.1 °C min −1 . Cryogenic focusing of desorbed species was required to achieve resolution of antimony species. The optimized SPME–GC–MS method was applied to the analysis of headspace gases from cultures of Cryptococcus humicolus incubated with inorganic antimony(III) and (V) substrates. The headspace gases from biphasic (aerobic–anaerobic) biomass‐concentrated culture incubations revealed the presence of SbH 3 , Me 2 Sb and Me 3 Sb. Stibine was the major antimony species detected in cultures amended with inorganic antimony(V). Me 3 Sb was the sole volatile antimony species detected when cultures were amended with antimony(III). Copyright © 2002 John Wiley & Sons, Ltd.