Medical Aspects of Chemical Warfare (2008) - The Black Vault

Medical Aspects of Chemical WarfareTable 22-9Analytical Methods Used to Verify Exposure to Sulfur Mustard in BiomedicalSamplesSample Matrix Biomarker Sample Preparation Analytical Method LODUrine, blood, TDG enzyme incubation, derivatization Negative ion chemical ~ 1 ng/mL 1plasmaionization GC-MSUrine TDG enzyme incubation, derivatization Electron impact GC-MS ~ 1 ng/mL 2Urine TDG, TDG-sulfoxide TiCl 3reduction, derivatization Negative ion chemical < 1 ng/mL 3ionization GC-MS-MSUrine TDG, TDG-sulfoxide Enzyme incubation, TiCl 3reduction, Positive ion chemical 0.5 ng/mL 4derivatizationionization GC-MSUrine TDG-sulfoxide Derivatization negative ion chemical 2 ng/mL 5ionization GC-MSUrine SBMTE TiCl 3reduction positive ion chemical 0.1 ng/mL 6ionization GC-MS-MSUrine SBmte tiCl 3reduction positive ion chemical 0.04 ng/mL 7ionization GC-MS-MSUrine MSMTESE SPE cartridge extraction positive ion electrospray 0.1–0.5 ng/mL 8lc-MS-MSUrine SBMSE SPE cartridge extraction positive ion electrospray 0.1–0.5 ng/mL 8lc-MS-MSUrine Bis-(N-acetyl cysteine) SPE cartridge extraction negative ion electrospray 0.5–1 ng/mL 9conjugatelc-MS-MSBlood Hemoglobin valine Globin isolation, valine cleavage by Negative ion chemical 100 nM wholeadduct edman degradation, derivatization ionization GC-MS blood exposureBlood Hemoglobin valine Globin isolation, valine cleavage by High-resolution negative 0.5 pmoladduct edman degradation ion chemical ionization adduct/mL 12GC-MSBlood Hemoglobin histidine Acid hydrolysis of globin, Positive ion electrospray Not reported 12adduct derivatization lc-MS-MSBlood Hemoglobin histidine Acid hydrolysis of globin, Positive ion electrospray 10 µM wholeadduct derivatization lc-MS-MS blood exposure13Plasma Albumin cysteine Albumin isolation, pronase Positive ion electrospray 10 nM wholeadduct digestion lc-MS-MS blood exposure14,15Blood, plasma Protein adducts Protein precipitation, alkaline Negative ion chemical 25 nM plasmahydrolysis, derivatization, SPE ionization GC-MS exposure 16extractionBlood DNA adducts WBC isolation, lysis, extraction, Immunuslotblot assay 50 nM wholetreatment with RNase andblood expoproteinaseK sure 17Skin dna adducts Epidermal layer isolation, lysis, Immunuslotblot assay 1 sec skinextraction, treatment with RNaseexposure toand proteinase Ksaturatedvapor 17Skin Keratin adducts Alkaline hydrolysis, derivatization LC-radiometric detector Not reported 18(Table 22-9 continues)714