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有机锡、铅、汞检测试剂——四乙基硼酸钠

有机锡、有机铅和有机汞对人类及动植物有毒性,因此食品、纺织、玩具、环境等领域都需要针对这些化合物进行检测,以保障人们的健康安全。

目前,针对这些化合物已开发出多种检测及定量分析方法,其中大部分基于气相色谱(GC),并结合各种灵敏性且具高选择性的检测方法,例如:原子吸收光谱(AAS),原子发射光谱(AES),脉冲火焰光度检测(PFPD)和质谱(MS)等。基于气相色谱(GC)的检测方法,需对分析物先进行衍生化以增加其挥发性, 同时衍生化还可防止分析过程中(尤其是检测阶段)的干扰。专一且可定量的衍生化方法可避免分析物的损失或降解,对分析结果至关重要。常用的方法是使用格氏试剂四乙基硼酸钠进行氢化和烷基化。

四乙基硼酸钠是理想的衍生化试剂


因其对含有机金属的水溶性样品进行衍生化时,将在原位进行反应,从而避免了其他操作步骤。乙基化产物的收率取决于与金属相连烷基的取代度及类型、pH值和反应时间。例如:有机锡化合物检测合适的pH值为4-5。

另外,由于样品中含有的其他金属也会参与反应消耗试剂,因此必须使用过量的NaBEt4[1]
除GC外,四乙基硼酸钠衍生化还可用于多种光谱检测方法,并应用于多种环境样品中有毒有机金属物质分析,示例如下:

  • Devos, Christophe, Luc Moens, and Pat Sandra. "Determination of the acaricide fenbutatin oxide in water samples by automated headspace‐SPME‐GC/MS." Journal of separation science 28, no. 7 (2005): 665-668.

  • Orellana-Velado, Néstor Guillermo, Rosario Pereiro, and Alfredo Sanz-Medel. "Solid phase microextraction gas chromatography-glow discharge-optical emission detection for tin and lead speciation." Journal of Analytical Atomic Spectrometry 16, no. 4 (2001): 376-381.

  • Perna, Lorenzo, Angela LaCroix-Fralish, and Stefan Stürup. "Determination of inorganic mercury and methylmercury in zooplankton and fish samples by speciated isotopic dilution GC-ICP-MS after alkaline digestion." Journal of Analytical Atomic Spectrometry 20, no. 3 (2005): 236-238.

  • Larsson, Tom, Erik Björn, and Wolfgang Frech. "Species specific isotope dilution with on line derivatisation for determination of gaseous mercury species." Journal of analytical atomic spectrometry 20, no. 11 (2005): 1232-1239.

  • Bowles, Karl C., Simon C. Apte, and Leigh T. Hales. "Determination of butyltin species in natural waters using aqueous phase ethylation and off-line room temperature trapping." Analytica chimica acta 477, no. 1 (2003): 103-111.

  • Clark, Steven, and Peter J. Craig. "The use of sodium tetraethylborate for the derivatization and analysis of selenium containing compounds." Microchimica Acta 109, no. 1-4 (1992): 141-144.

  • Mota, J. Pablo Valles, M. Rosario Fernández de la Campa, and Alfredo Sanz-Medel. "Merging zones flow injection for the determination of ultratraces of bismuth by volatile species generation atomic absorption spectrometry using sodium tetraethylborate (III)." Journal of Analytical Atomic Spectrometry 13, no. 5 (1998): 431-435.

  • Ndungu, Kuria, and Lennart Mathiasson. "Microporous membrane liquid–liquid extraction technique combined with gas chromatography mass spectrometry for the determination of organotin compounds." Analytica chimica acta 404, no. 2 (2000): 319-328.


参考文献:
  1. Morabito, Roberto, Paolo Massanisso, and Philippe Quevauviller. "Derivatization methods for the determination of organotin compounds in environmental samples." TrAC Trends in Analytical Chemistry 19, no. 2-3 (2000): 113-119.

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