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顶空固相微萃取结合气相色谱-脉冲火焰光度检测法对人尿中有机锡化合物的形态分析

Speciation analysis of organotin compounds in human urine by headspace solid-phase micro-extraction and gas chromatography with pulsed flame photometric detection.

作者信息

Valenzuela Aníbal, Lespes Gaëtane, Quiroz Waldo, Aguilar Luis F, Bravo Manuel A

机构信息

Laboratorio de Química Analítica y Ambiental, Instituto de Química, Pontificia Universidad Católica de Valparaíso, Avenida Universidad 330, Curauma, Valparaíso, Chile.

Laboratoire de Chimie Analytique Bio Inorganique et Environment, IPREM, Université de Pau et des Pays de l׳Adour, Avenue de l׳Université, 64013 Pau, France.

出版信息

Talanta. 2014 Jul;125:196-203. doi: 10.1016/j.talanta.2014.02.054. Epub 2014 Feb 28.

DOI:10.1016/j.talanta.2014.02.054
PMID:24840433
Abstract

A new headspace solid-phase micro-extraction (HS-SPME) method followed by gas chromatography with pulsed flame photometric detection (GC-PFPD) analysis has been developed for the simultaneous determination of 11 organotin compounds, including methyl-, butyl-, phenyl- and octyltin derivates, in human urine. The methodology has been validated by the analysis of urine samples fortified with all analytes at different concentration levels, and recovery rates above 87% and relative precisions between 2% and 7% were obtained. Additionally, an experimental-design approach has been used to model the storage stability of organotin compounds in human urine, demonstrating that organotins are highly degraded in this medium, although their stability is satisfactory during the first 4 days of storage at 4 °C and pH=4. Finally, this methodology was applied to urine samples collected from harbor workers exposed to antifouling paints; methyl- and butyltins were detected, confirming human exposure in this type of work environment.

摘要

已开发出一种新的顶空固相微萃取(HS-SPME)方法,随后采用气相色谱-脉冲火焰光度检测(GC-PFPD)分析,用于同时测定人尿中的11种有机锡化合物,包括甲基、丁基、苯基和辛基锡衍生物。通过对添加了不同浓度水平所有分析物的尿液样本进行分析,验证了该方法,回收率高于87%,相对精密度在2%至7%之间。此外,采用实验设计方法对有机锡化合物在人尿中的储存稳定性进行建模,结果表明有机锡在这种介质中极易降解,不过在4℃和pH=4的条件下储存的前4天,其稳定性令人满意。最后,将该方法应用于从接触防污涂料的港口工人收集的尿液样本;检测到了甲基锡和丁基锡,证实了在这类工作环境中人体会接触到这些物质。

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