Department of Analytical Chemistry, Faculty of Chemistry, Regional Campus of International Excellence Campus Mare Nostrum, University of Murcia, E-30071 Murcia, Spain.
J Chromatogr A. 2013 Mar 1;1279:1-6. doi: 10.1016/j.chroma.2012.12.067. Epub 2013 Jan 8.
A method based on headspace sorptive extraction (HSSE) in combination with thermal desorption-gas chromatography-mass spectrometry (TD-GC-MS) has been developed for the simultaneous determination of six organotin compounds (OTCs), corresponding to mono- and di-substituted methyltin, butyltin and octyltin species. Several parameters affecting both the headspace extraction and thermal desorption steps were carefully optimized using multivariate designs. Analytes were derivatized by in situ ethylation with sodium tetraethylborate. The optimized method was applied to the analysis of water samples of different origins, as well as to checking the migration of the studied compounds from commercially available plastic containers to the adequate liquid simulant. Quantification was carried out against aqueous calibration curves using diphenyltin as internal standard, providing detection limits of between 1.7 and 7.0 ng(Sn) L(-1), depending on the compound, and repeatabilities lower than 10% in terms of relative standard deviation. The applicability of the method was assessed by means of recovery studies and satisfactory values for all compounds were attained. The release of OTCs from the tested packages to the liquid simulant was confirmed, concentrations as high as 2.4 μg(Sn) L(-1) being found for dioctyltin. Even though the proposed method was developed for organotin halides, its application to an organotin ester shows its suitability for determining these compounds in migration assays.
一种基于顶空固相萃取（HSSE）与热解吸-气相色谱-质谱联用（TD-GC-MS）的方法已经被开发出来，用于同时测定六种有机锡化合物（OTCs），包括单取代和二取代的甲基锡、丁基锡和辛基锡。通过多元设计，对影响顶空萃取和热解吸步骤的多个参数进行了仔细优化。分析物通过原位与四乙基硼酸钠进行乙基化衍生化。优化后的方法被应用于不同来源水样的分析，以及检查研究化合物从市售塑料容器向适当的液体模拟物的迁移情况。使用二苯基锡作为内标，通过水相校准曲线进行定量，根据化合物的不同，检测限在 1.7 到 7.0ng(Sn)L(-1)之间，相对标准偏差的重复性低于 10%。通过回收率研究评估了该方法的适用性，所有化合物均获得了令人满意的结果。证实了 OTCs 从测试包装向液体模拟物的释放，二辛基锡的浓度高达 2.4μg(Sn)L(-1)。尽管该方法是针对有机锡卤化物开发的，但将其应用于有机锡酯表明其适用于在迁移试验中测定这些化合物。
