Department of Environmental Chemistry, Institute of Environmental Assessment and Water Research, IDAEA-CSIC, Jordi Girona, 18-26, E-08034 Barcelona, Spain.
J Chromatogr A. 2009 Dec 18;1216(51):8828-34. doi: 10.1016/j.chroma.2009.10.043. Epub 2009 Oct 20.
A method for trace level determination of organomercury species in different biota matrixes by using aqueous-phase propylation followed by headspace solid-phase microextraction (HS-SPME) and gas chromatography (GC) coupled to pyrolysis-atomic fluorescence spectrometry (Py-AFS) detection has been optimized. To maximize peak area and symmetry factors of methylmercury (MeHg) and ethylmercury (EtHg) analyzed as propyl derivatives, carrier and make-up flow rates were optimized by a user-defined experimental design. A multiple response simultaneous optimization was applied using the desirability function to achieve global optimal operating conditions. They were attained at 2 and 6 mL min(-1) as carrier and make-up gas flow rates, respectively. In addition, pyrolyser temperature was also optimized, yielding the best value at 750 degrees C. Limits of detection and quantification at the optimum conditions were 0.04 ng g(-1) and 0.13 ng g(-1) for both, MeHg and EtHg. The developed analytical procedure was validated with a certified reference material (DORM-2) and applied to the determination of organomercury incurred in waterfowl egg and fish samples.
一种通过水相丙基化结合顶空固相微萃取（HS-SPME）和气相色谱（GC）与裂解-原子荧光光谱法（Py-AFS）联用检测来测定不同生物基质中有机汞形态的痕量方法已得到优化。为了使作为丙基衍生物分析的甲基汞（MeHg）和乙基汞（EtHg）的峰面积和对称因子最大化，通过用户定义的实验设计优化了载气流速和补充气流速。使用可接受性函数进行多响应同时优化，以达到全局最佳操作条件。分别在载气流速和补充气体流速为 2 和 6 mL min(-1) 时达到最佳条件。此外，还优化了热解器温度，在 750°C 时得到最佳值。在最佳条件下，MeHg 和 EtHg 的检测限和定量限均为 0.04 ng g(-1) 和 0.13 ng g(-1)。该分析方法已用认证参考物质（DORM-2）进行了验证，并应用于测定水禽蛋和鱼类样品中的有机汞。
