PubMed · 8947809
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D Morgan-Jones, T Hodgetts. 1996. Sarin.. https://doi.org/10.1136/emj.13.6.431-c
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A method of detecting signature methylphosphonic acid (MPA) breakdown products of V and G nerve agents in environmental samples was developed using capillary ion electrophoresis with conductivity detection. The electrolyte (30 mM L-histidine, 30 mM 2-(N-morpholino)ethanesulfonic acid, 0.7 mM tetradecyltrimethylammonium hydroxide, and 0.03 weight% Triton X-100) allowed baseline separation of MPA, ethyl methylphosphonic acid (EMPA), isopropyl methylphosphonic acid (IMPA), and pinacolyl methylphosphonic acid (PMPA) in less than 10 min. Detector response was linear in the 6-60 micrograms/ml concentration range (correlation coefficient = 0.99) with a detection limit around 6 micrograms/ml. The application of this method for screening MPA, EMPA, IMPA, and PMPA in surface water, groundwater, and soil extracts is demonstrated.
Quantitative methods have been developed for the analysis of chemical warfare agent degradation products in reaction masses using capillary electrophoresis (CE). This is the first report of a systematic validation of a CE-based method for the analysis of chemical warfare agent degradation products in agent neutralization matrixes (reaction masses). After neutralization with monoethanolamine/water, the nerve agent GB (isopropyl methylphosphonofluoridate, Sarin) gives isopropyl methylphosphonic acid (IMPA) and O-isopropyl O'-(2-amino)ethyl methylphosphonate (GB-MEA adduct). The nerve agent GD (pinacolyl methylphosphonofluoridate, Soman), [pinacolyl = 2-(3,3-dimethyl)butyl] produces pinacolyl methylphosphonic acid (PMPA) and O-pinacolyl O'-(2-amino)ethyl methylphosphonate (GD-MEA adduct). The samples were prepared by dilution of the reaction masses with deionized water before analysis by CE/indirect UV detection or CE/conductivity detection. Migration time precision was less than 4.0% RSD for IMPA and 5.0 RSD for PMPA on a day-to-day basis. The detection limit for both IMPA and PMPA is 100 micrograms/L; the quantitation limit for both is 500 micrograms/L. For calibration standards, IMPA and PMPA gave a linear response (R2 = 0.9999) over the range 0.5-100 micrograms/mL. The interday precision RSDs were 1.9, 1.0, and 0.7% for IMPA at 7.5, 37.5 and 75.0 micrograms/mL, respectively. Corresponding values for PMPA (again, RSD) were 2.9, 1.1, and 1.0% at 7.5, 37.5 and 87.5 micrograms/mL, respectively, as before. Analysis accuracy was assessed by spiking actual neutralization samples with IMPA or PMPA. For IMPA, the seven spike levels used ranged from 20 to 220% of the IMPA background level, and the incremental change in the found IMPA level ranged from 86 to 99 % of the true spiking increment (R2 = 0.9987 for the linear regression). For PMPA, the five spike levels ranged from 10 to 150% of the matrix background level, and similarly, the accuracy obtained ranged from 95 to 97% of the true incremental value (R2 = 0.9999 for the linear regression).
Methods for the identification of chemical warfare agents, toxins, bioregulators and related products are frequently reported in literature. These methods are often based on instrumental analysis using chromatography (gas and liquid) and mass spectrometry. Here, these instrumental techniques are discussed in several applications, new developments and trends based on a review of the literature published since 1990. Apart from new instrumental developments, it is shown that modern analytical chemistry can be successfully applied to perform identification in the broad field of analytes ranging from chemical to biological warfare agents.