Lewisite Metabolites in Urine by Solid Phase Extraction-Dual Column Reversed-Phase Liquid Chromatography-Isotope Dilution Tandem Mass Spectrometry.
Autor: | Palcic JD; Florida Department of Health, Bureau of Public Health Laboratories, 1217 N. Pearl St, Jacksonville, FL 32202, USA alcic@flhealth.gov., Donovan SF; NMS Labs, 3701 Welsh Rd, Willow Grove, PA 19090, USA., Jones JS; Florida Department of Health, Bureau of Public Health Laboratories, 1217 N. Pearl St, Jacksonville, FL 32202, USA., Flagg EL; Florida Department of Health, Bureau of Public Health Laboratories, 1217 N. Pearl St, Jacksonville, FL 32202, USA., Salonga RA; Florida Department of Health, Bureau of Public Health Laboratories, 1217 N. Pearl St, Jacksonville, FL 32202, USA., Mock WE; Florida Department of Health, Bureau of Public Health Laboratories, 1217 N. Pearl St, Jacksonville, FL 32202, USA., Asirvatham VS; Florida Department of Health, Bureau of Public Health Laboratories, 1217 N. Pearl St, Jacksonville, FL 32202, USA. |
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Jazyk: | angličtina |
Zdroj: | Journal of analytical toxicology [J Anal Toxicol] 2016 Jul; Vol. 40 (6), pp. 419-26. Date of Electronic Publication: 2016 Jun 23. |
DOI: | 10.1093/jat/bkw049 |
Abstrakt: | Lewisite (2-chlorovinyldichloroarsine) is a chemical warfare agent developed during World War I. A quantitative method using solid phase extraction (SPE) followed by dual column liquid chromatography (LC)-isotope dilution tandem mass spectrometry (MS-MS) was developed for the determination of (2-chlorovinyl)arsonic acid (CVAOA), a metabolite of Lewisite, in human urine. The sample was treated with hydrogen peroxide to oxidize any (2-chlorovinyl)arsonous acid (CVAA) that remained in the trivalent arsenic oxidation state. There was 1.19% (arsenic purity) of bis-(2-chlorovinyl)arsinic acid (BCVAOA), a minor Lewisite metabolite, in the stock CVAA material. The high-throughput method qualitatively assessed BCVAOA simultaneously utilizing normal-phase silica SPE followed by reversed-phase C18 LC for an orthogonal separation. The chromatographic method results in a 5.8-min cycle time with adequate retention (k' = 2.4) of CVAOA. The mass spectrometer was operated in positive electrospray ionization mode with quantitative m/z 186.9→61.0 and confirmation 186.9→91.0 mass transitions. This selective method demonstrated linearity, accuracy and reproducibility for the clinically relevant calibration range (25-3,200 µg/L as CVAA). The method detection limit was 3.3 µg/L as CVAA from a 10 µL injection. This LC-MS-MS emergency response method has a throughput of >240 samples (2.5 extracted 96-well plates) per day. (© The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.) |
Databáze: | MEDLINE |
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