尿中游离碘与硫氰化物的固相微萃取

Solid Phase Microextraction for free Iodide and Thiocyan in Urine

目的 用衍生化和固相微萃取技术从尿中提取游离碘和硫氰酸盐。二者在碱性条件下与五氟卞基溴反应 ,生成五氟卞基衍生物。方法 在 80℃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 5min。用 1,3,5 -三溴苯作内标 ,气 /质联用仪测定。用选择离子m/z181(五氟卞基 )和m/z314(内标 )的峰面积比定量。结果 尿中检测浓度可达 0 0 1μg/ml。

Objective In the paper,solid phase microextraction(SPME)and derivatization with pentafluorobenzylbromide for free iodide and thiocyan in urine was presanted.Methods The derivatives of free iodide and thiocyan were extracted for 25 min at the condition of 80℃ temperature by a polydimethylsiloxane fiber.1,3,5-tribromobenzene(IS) was used as an internal standard.GC/MS was used for analysis.The ions at m/z 181(both of the derivatives)and m/z 312(IS) in the selected ion monitoring chromatograms were selected for quantitation. Results The compounds were detectable at least 0.01μg/ml.Conclusion This method would be demonstrated to be simple and useful.