硫化氢衍生化固相微萃取分析研究

Solid phase microextraction and derivatization of sulfide in blood with pentaf luorobenzylbromide

用衍生化和固相微萃取技术从血中提取硫化氢。硫化氢在碱性条件下与五氟卞基溴反应 ,生成五氟卞基硫醚的衍生物。在 45℃条件下用 10 0 μm聚二甲基硅氧烷萃取头以顶空方式提取 2 0min。用 1,3 ,5 三溴苯作内标 ,气 质联用仪测定。用分子离子m z 3 94(五氟卞基硫醚 )和m z 3 12 (内标 )的峰面积比定量。血中检测浓度可达 0 0 1μg g。通过硫化氢中毒案例的实际测定证明 。

Solid phase microextraction (SPME) and derivatization with pentafluor obenzylbromide for sulfide in blood was presented in the paper. The derivative o f sulfide was extracted for 20 min at the condition of room temperatrue by a pol ydimethylsiloxane fiber. 1,3,5-tribromobenzene (IS) was used as an internal sta n derd. GC/MS was used for analysis. The ions at m/z 394 (derivative of sulfide) a nd m/z 312 (IS) in the selected ion minitoring chromatograms were selected for q uantitation. The compound was detectable at least 0.01μg/ml. By the determinati on in poisoning blood, this method would be demonstrated to be simple.