分析化学Issue(7)：980-984,5.DOI:10.11895/j.issn.0253-3820.131223
同位素稀释气相色谱-质谱联用法监测芥子气染毒家兔尿液中的硫二甘醇
Monitoring Urine Thiodiglycol after Rabbit Skin Exposure to Sulfur Mustard Based on Highly-sensitive Isotope Dilution Gas Chromatography-Mass Spectrometry
摘要
Abstract
A sensitive determination method for sulfur mustard ( HD ) metabolites thiodiglycol ( TDG ) in rabbit urine was established and validated using isotope dilution negative ion chemical ionization ( NICI) gas chromatography-mass spectrometry ( GC-MS ) , in which deuterated thiodiglycol ( TDG-d8 ) was used as internal standard. Two solid-phase extraction ( SPE) steps were established and optimized in order to reduce the interfering backgrounds, one was used to extract thiodiglycol ( TDG ) from urine with self-assemblied Florisil SPE cartridges, another cleaning treatment of the by-products after pentafluorobenzoyl chloride (PFBZ) derivatization. The results showed that the limits of detection quantitation of this method were 0. 1 and 0. 3 μg/L, respectively. The exposure time-response relationship and exposure dose-response relationship of TDG in rabbit urine were studied after rabbit skin exposure to sulfur mustard (HD, 0. 02-0. 15 LD50). The TDG levels in the rabbit urine increased rapidly during the first day after application and then decreased over time for all dosage groups. A secondary release was also noted for the high-dose group, and the duration of high TDG excretion levels was correlated positively with the HD dosage levels. We thus concluded that abnormally high levels of TDG in urine could be used as a clear diagnostic indicator of HD exposure.关键词
生物标志物/硫二甘醇/固相萃取/芥子气/气相色谱-质谱联用Key words
Biomarkers/Thiodiglycol/Solid-phase extraction/Sulfur mustard/Gas chromatography/mass spectrometry引用本文复制引用
聂志勇,张雅姣,吴弼东,闫珑,冯建林,刘勤,谢剑炜..同位素稀释气相色谱-质谱联用法监测芥子气染毒家兔尿液中的硫二甘醇[J].分析化学,2014,(7):980-984,5.基金项目
本文系国家科技部重大专项基金(No.2012ZX09301003-001-010)资助项目@@@@This work was supported by the Minstry of National Science and Technology Major Special Fund (No.2012ZX09301003-001-010) （No.2012ZX09301003-001-010）
