Viñas Pilar, López-García Ignacio, Merino-Meroño Beatriz, Campillo Natalia, Hernández-Cordóba Manuel
Department of Analytical Chemistry, Faculty of Chemistry, University of Murcia, E-30071 Murcia, Spain.
J Environ Monit. 2004 Apr;6(4):262-6. doi: 10.1039/b312778h. Epub 2004 Feb 11.
Liquid chromatography with hydride generation atomic absorption spectrometry as the detection system was applied to the separation and determination of inorganic tin, tributyltin, dibutyltin, monobutyltin, diphenyltin and monophenyltin. A reversed phase C18 column and a methanol/water/acetic acid (70:27:3, v/v/v) mixture containing 0.05%(v/v) triethylamine and 0.1%(w/v) tropolone as the mobile phase (isocratic elution) were used. Extraction of organotins from the samples was carried out using methanol containing 0.05%(w/v) tropolone, a process that was repeated twice. The supernatants were shaken with water and dichloromethane in a separating funnel and the organic phase was collected and evaporated to dryness. When the method was applied to the speciation of tin in fresh and canned mussels, no organotins above the detection limits were identified in any of the samples, inorganic tin being the only species detected. The reliability of the procedure was checked by analyzing the total tin content of the samples by electrothermal atomic absorption spectrometry and by speciation of tin in a certified reference material, mussel tissue (CRM 477). The method can be used for environmental monitoring of organotins contaminated samples.
采用液相色谱-氢化物发生原子吸收光谱法作为检测系统,对无机锡、三丁基锡、二丁基锡、单丁基锡、二苯基锡和单苯基锡进行分离和测定。使用反相C18柱,以甲醇/水/乙酸(70:27:3,v/v/v)混合液为流动相,其中含有0.05%(v/v)三乙胺和0.1%(w/v)托酚酮(等度洗脱)。采用含有0.05%(w/v)托酚酮的甲醇从样品中萃取有机锡,该过程重复两次。将上清液在分液漏斗中与水和二氯甲烷振荡,收集有机相并蒸发至干。当该方法应用于新鲜贻贝和罐装贻贝中锡的形态分析时,在任何样品中均未鉴定出高于检测限的有机锡,仅检测到无机锡。通过电热原子吸收光谱法分析样品中的总锡含量以及对贻贝组织标准物质(CRM 477)中的锡进行形态分析,检验了该方法的可靠性。该方法可用于受有机锡污染样品的环境监测。