Vidal J L Martínez, Vega A Belmonte, Arrebola F J, González-Rodríguez M J, Sánchez M C Morales, Frenich A Garrido
Department of Analytical Chemistry, University of Almería, 04120 Almería, Spain.
Rapid Commun Mass Spectrom. 2003;17(18):2099-106. doi: 10.1002/rcm.1152.
A fast method for the determination of eight organotin compounds (OTs), monobutyltin (MBT), dibutyltin (DBT), tributyltin (TBT), tetrabutyltin (TeBT), monophenyltin (MPhT), diphenyltin (DPhT), triphenyltin (TPhT) and tetraphenyltin (TePhT), in water, sediments and mussels, was developed using low-pressure gas chromatography/tandem mass spectrometry (LPGC/MS/MS). The method is based on sodium diethyldithiocarbamate (DDTC) complexation of the ionic organotins, followed by extraction of the target matrices and derivatization by a Grignard reagent, as described in a previously published method for water samples. Solid-phase extraction was selected as extraction method from water samples after comparison with liquid-liquid extraction, but extraction of the OTs from sediment and mussel samples was performed using toluene. Matrix-matched calibration standards were used to minimize matrix effects. The analytical process was validated by the analysis of spiked blank samples. Performance characteristics such as linearity, detection limit (LOD), quantitation limit (LOQ), precision, and recovery were determined. Recoveries of OTs in spiked matrices ranged from 86-108% in water and from 78-110% in sediments and mussels, with precision values lower than 18%. Detection limits ranged from 0.1-9.6 ng L(-1) in water, and 0.03-6.10 microg kg(-1) in the other matrices. The present implementation of LPGC rather than conventional capillary GC permitted use of large-volume injection and reduced analysis time by a factor of two. The proposed methodology was applied to the determination of OTs in real samples of water, marine sediments and mussels from the west coast of the Mediterranean Sea (Spain).
采用低压气相色谱/串联质谱法（LPGC/MS/MS）开发了一种快速测定水、沉积物和贻贝中8种有机锡化合物（OTs）的方法，这8种化合物分别为单丁基锡（MBT）、二丁基锡（DBT）、三丁基锡（TBT）、四丁基锡（TeBT）、单苯基锡（MPhT）、二苯基锡（DPhT）、三苯基锡（TPhT）和四苯基锡（TePhT）。该方法基于离子型有机锡与二乙基二硫代氨基甲酸钠（DDTC）络合，然后萃取目标基质，并通过格氏试剂进行衍生化，如先前发表的水样分析方法所述。与液液萃取相比，选择固相萃取作为水样的萃取方法，但沉积物和贻贝样品中的OTs萃取采用甲苯进行。使用基质匹配校准标准来最小化基质效应。通过分析加标空白样品对分析过程进行验证。测定了线性、检测限（LOD）、定量限（LOQ）、精密度和回收率等性能特征。加标基质中OTs的回收率在水中为86% - 108%，在沉积物和贻贝中为78% - 110%，精密度值低于18%。检测限在水中为0.1 - 9.6 ng L⁻¹，在其他基质中为0.03 - 6.10 μg kg⁻¹。采用LPGC而非传统的毛细管GC，允许使用大体积进样，并将分析时间缩短了一半。所提出的方法应用于测定地中海西部海岸（西班牙）水、海洋沉积物和贻贝的实际样品中的OTs。
