Oostdijk J P, Degenhardt C E A M, Trap H C, Langenberg J P
Varian B.V., Department R&D Consumable Products, Herculesweg 8, 4338 PL Middelburg, The Netherlands.
J Chromatogr A. 2007 May 25;1150(1-2):62-9. doi: 10.1016/j.chroma.2006.08.053. Epub 2006 Sep 11.
An improved method is presented for the trace analysis of sulfur mustard (HD) in biological samples, such as blood and tissue from laboratory animals. Using the internal standard method and liquid-liquid extraction with ethyl acetate, up to 400 microL of the extract was injected by thermal desorption from Tenax and analyzed by two-dimensional GC-MS/EI in SIM mode. The analysis was compared with a direct GC injection. Reversed thermal desorption was used as a tool for handling heavily contaminated (fat) samples, thus preventing contamination of the injection system and pre-column. A successful analytical configuration has been set up for the bioanalysis of HD at the low, toxicologically relevant pM level. A detection limit of 10 pg mL(-1) blood or pg g(-1) tissue of sulfur mustard (S/N=3) was established by using this configuration.
本文提出了一种改进方法，用于对生物样品（如实验动物的血液和组织）中的硫芥（HD）进行痕量分析。采用内标法和乙酸乙酯液液萃取，通过Tenax热脱附进样高达400 μL的萃取液，并采用二维气相色谱-质谱/电子轰击电离（GC-MS/EI）在选择离子监测（SIM）模式下进行分析。将该分析方法与直接气相色谱进样法进行了比较。反向热脱附用作处理严重污染（富含脂肪）样品的工具，从而防止进样系统和预柱受到污染。已建立了一种成功的分析配置，用于在低至毒理学相关的皮摩尔（pM）水平下对硫芥进行生物分析。使用该配置确定了硫芥在血液中的检测限为10 pg mL⁻¹或在组织中的检测限为10 pg g⁻¹（信噪比S/N = 3）。
