Solid phase microextraction(SPME) can be effectively used to extract volatile and semivoltaile organic compounds from different environmental matrix. In this paper, we utilize headspace-SPME technique combined with capillary gas chromatography (CGC) and a laboratory modified flame photometric detector using quartz surfaceinduced luminescence (QSIL-FPD) for analyzing butyltin compounds in sediments. The detection limits of mono-,di-, and tri-butyltin compounds, based on the signal equal to 3 times the baseline noise are 16.9 ng/g, 1.58 ng/g adn 0.17 ng/g, respectively.%固相微萃取可用于多种样品基体中挥发、半挥发性有机化合物的测定。将固相微萃取技术应用于底泥样品中丁基锡化合物的富集和萃取，以气相色谱分离结合表面发射火焰光度检测器检测，方法灵敏、快速，一丁、二丁、三丁基锡的检测限可达16.9、1.58和0.17 ng/g。
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