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Determination of organotin compounds by headspace solid-phase microextraction-gas chromatography-pulsed flame-photometric detection (HS-SPME-GC-PFPD)

机译:顶空固相微萃取-气相色谱-脉冲火焰光度检测法(HS-SPME-GC-PFPD)测定有机锡化合物

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摘要

A method based on Headspace solid-phase microextraction (HS-SPME, with a 100 mu m PDMS-fiber) in combination with gas-chromatography and pulsed flame-photometric detection (GC-PFPD) has been investigated for simultaneous determination of eight organotin compounds. Monobutyltin (MBT), dibutyltin (DBT), tributyltin (TBT), monophenyltin (MPhT), and the semi-volatile diphenyltin (DPhT), triphenyltin (TPhT), monooctyltin (MOcT), and dioctyltin (DOcT) were determined after derivatization with sodium tetraethylborate. The conditions used for the extraction and preconcentration step were optimised by experimental design methodology. Tripropyltin (TPrT) and diheptyltin (DHepT) were used as internal standards for quantification of volatile and semi-volatile organotin compounds, respectively. The analytical precision (RSD) for ten successive injections of a standard mixture containing all the organic tin compounds ranged between 2 and 11%. The limits of detection for all the organotin compounds were sub ng (Sn) L-1 in water and close to ng (Sn) kg(-1) in sediments. The accuracy of the method was evaluated by analysis of two certified reference material (CRM) sediment samples. The HS-SPME-GC-PFPD was then applied to the analysis of three harbour sediment samples. The results showed that headspace SPME is an attractive tool for analysis of organotin compounds in solid environmental matrices.
机译:研究了一种基于顶空固相微萃取(HS-SPME,PDMS纤维为100微米)结合气相色谱和脉冲火焰光度检测(GC-PFPD)的方法,用于同时测定8种有机锡化合物。丁腈锡(MBT),二丁基锡(DBT),三丁基锡(TBT),单苯基锡(MPhT)和半挥发性二苯基锡(DPhT),三苯基锡(TPhT),单辛基锡(MOcT)和二辛基锡(DOcT)在四乙基硼酸钠。通过实验设计方法优化了用于提取和预浓缩步骤的条件。三丙基锡(TPrT)和二庚基锡(DHepT)分别用作定量挥发性和半挥发性有机锡化合物的内标。十次连续进样包含所有有机锡化合物的标准混合物的分析精度(RSD)在2%至11%之间。所有有机锡化合物的检出限为水中的ng(Sn)L-1和沉积物中的接近ng(Sn)kg(-1)。该方法的准确性是通过分析两个认证的参考物质(CRM)沉积物样品来评估的。然后将HS-SPME-GC-PFPD用于三个港口沉积物样品的分析。结果表明,顶空SPME是用于分析固体环境基质中有机锡化合物的有吸引力的工具。

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