Dpto Ingeniería Química, Universidad de Valencia, Doctor Moliner 50, 46100 Burjassot, Valencia, Spain.
Talanta. 2010 Mar 15;80(5):1888-93. doi: 10.1016/j.talanta.2009.10.039. Epub 2009 Oct 24.
Triethyltin, tributyltin, diphenyltin and triphenyltin were selected as model compounds. The method is based on in situ ethylation and simultaneous headspace-solid-phase microextraction (HS-SPME) and gas chromatographic-mass spectrometry analysis (GC-MS). The extraction procedure was optimized studying some variables such as reaction time, salinity, sample volume and headspace volume. SPME-GC-MS and SPME-GC-FID techniques were compared; quality assurance parameters such as sensitivity, selectivity and precision were established. The proposed procedure showed limits of detection between 0.025 and 1ng/L. The linearity was in the 0.025-5000 ng/L range. The precision expressed as relative standard deviations (RSD), were below 20%. Real wastewaters and seawaters were analyzed. The method permits controlling legislated annual average values.
三乙基锡、三丁基锡、二苯基锡和三苯基锡被选为模型化合物。该方法基于原位乙基化和同时顶空固相微萃取（HS-SPME）和气相色谱-质谱分析（GC-MS）。通过研究反应时间、盐度、样品体积和顶空体积等变量对萃取程序进行了优化。比较了 SPME-GC-MS 和 SPME-GC-FID 技术；建立了质量保证参数，如灵敏度、选择性和精密度。该方法的检出限在 0.025 和 1ng/L 之间。线性范围在 0.025-5000ng/L 之间。精密度以相对标准偏差（RSD）表示，低于 20%。对实际废水和海水进行了分析。该方法可以控制法定的年平均值。
