Quantitation of fluoride ion released sarin in red blood cell samples by gas chromatography-chemical ionization mass spectrometry using isotope dilution and large-volume injection.
A new method for measuring fluoride ion released isopropyl methylphosphonofluoridate (sarin, GB) in the red blood cell fraction was developed that utilizes an autoinjector, a large-volume injector port (LVI), positive ion ammonia chemical ionization detection in the SIM mode, and a deuterated stable isotope internal standard. This method was applied to red blood cell (RBC) and plasma ethyl acetate extracts from spiked human and animal whole blood samples and from whole blood of minipigs, guinea pigs, and rats exposed by whole-body sarin inhalation. Evidence of nerve agent exposure was detected in plasma and red blood cells at low levels of exposure. The linear method range of quantitation was 10-1000 pg on-column with a detection limit of approximately 2-pg on-column. In the course of method development, several conditions were optimized for the LVI, including type of injector insert, injection volume, initial temperature, pressure, and flow rate. RBC fractions had advantages over the plasma with respect to assessing nerve agent exposure using the fluoride ion method especially in samples with low serum butyrylcholinesterase activity.
Jakubowski
E M
EM
Research and Technology Directorate, U.S. Army ECBC, APG-EA, Edgewood, Maryland 21010, USA. edward.m.jakubowski@us.army.mil
McGuire
J M
JM
Evans
R A
RA
Edwards
J L
JL
Hulet
S W
SW
Benton
B J
BJ
Forster
J S
JS
Burnett
D C
DC
Muse
W T
WT
Matson
K
K
Crouse
C L
CL
Mioduszewski
R J
RJ
Thomson
S A
SA
D000818:Animals; D002619:Chemical Warfare Agents / Q000032:analysis* / Q000493:pharmacokinetics / Q000506:poisoning; D004305:Dose-Response Relationship, Drug; D004912:Erythrocytes / Q000737:chemistry*; D005459:Fluorides / Q000032:analysis*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006168:Guinea Pigs; D006801:Humans; D019570:Inhalation Exposure; D007474:Ion Exchange; D007553:Isotope Labeling; D051381:Rats; D017207:Rats, Sprague-Dawley; D012524:Sarin / Q000032:analysis* / Q000493:pharmacokinetics / Q000506:poisoning; D021241:Spectrometry, Mass, Electrospray Ionization / Q000295:instrumentation / Q000379:methods; D013552:Swine; D013556:Swine, Miniature
D002619:Chemical Warfare Agents; D012524:Sarin; D005459:Fluorides