Institute of Chemical Technologies and Analytics, Vienna University of Technology, Vienna, Austria.
J Sep Sci. 2012 May;35(9):1132-7. doi: 10.1002/jssc.201101041.
This work describes the development of a fast method for speciation analysis of triethyl-lead and tributyl-tin species in urine samples after in situ derivatization by tetraethyl- or tetrapropyl-borate reagents. The alkylation reaction is done in the aqueous and urine medium and the less-polar derivatives are extracted in hexane by liquid-liquid extraction. The species were extracted and the extract was efficiently collected from the aqueous phase after centrifugation. Finally, the organometallic species are separated by gas chromatography and determined from the emission signals of elemental lead and tin. Atomic lead and tin are formed from the organolead and organotin compounds during atomization of the column eluate in a microwave-induced helium plasma source. The simultaneous measurement of lead (Pb) at 405.780 nm and tin (Sn) at 303.419 nm was achieved by an atomic emission detector. Finally, the analytes were determined with satisfactory precision (<5%) and detection limits of 0.05 μg Pb/L and 0.48 μg Sn/L, respectively, when 10 mL of urine is extracted with 1 mL of hexane and 1 μL of extract is injected.
本工作描述了一种快速方法的发展，用于在原位衍生后通过四乙基或四丙基硼酸试剂在尿液样品中分析三乙基铅和三丁基锡的形态。烷基化反应在水相和尿液介质中进行，较非极性衍生物通过液 - 液萃取用正己烷萃取。在离心后，将物种从水相萃取并有效地从水相萃取。最后，通过气相色谱法分离有机金属物种，并从元素铅和锡的发射信号中进行测定。在微波诱导氦等离子体源中，柱洗脱液的原子化过程中，从有机铅和有机锡化合物中形成原子铅和原子锡。通过原子发射检测器实现了铅（Pb）在 405.780nm 和锡（Sn）在 303.419nm 的同时测量。最后，当用 1 毫升正己烷萃取 10 毫升尿液并注入 1 微升提取物时，用该方法分别以 0.05μg Pb/L 和 0.48μg Sn/L 的满意精密度（<5%）和检测限测定了分析物。
