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将分散液液微萃取(DLLME)与超高效液相色谱-串联质谱联用技术(UPLC-MS/MS)相结合,建立了环境水样中三苯基乙酸锡的测定方法。通过对萃取条件的优化,得到最佳条件:在5.0mL水样中加入30.0μL氯苯(萃取剂)和1.0mL丙酮(分散剂)的混合溶液,萃取1min,以4000r/min离心5min后吸出萃取剂氯苯直接进样分析。在优化条件下,三苯基乙酸锡的富集倍数为165倍,检出限为0.01μg/L(S/N=3),线性范围为0.05—5.0μg/L,线性相关系数为0.9991。本法应用于河水、湖水和井水样的分析,加标回收率在81.2%—106%之间,相对标准偏差在4.5%—7.8%之间(n=6)。
The determination of triphenyl tin acetate in environmental water samples was established by combining liquid chromatography-assisted liquid-liquid extraction (DLLME) and ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS / MS). The optimal conditions were obtained by adding the mixed solution of 30.0μL chlorobenzene (extractant) and 1.0mL acetone (dispersant) to 5.0mL water sample, extracting for 1min, then centrifuging at 4000r / min for 5min and then extracting Extractant chlorobenzene direct injection analysis. Under optimized conditions, the enrichment factor of triphenyltin acetate was 165-fold with a detection limit of 0.01μg / L (S / N = 3), linear range of 0.05-5.0μg / L and linear correlation coefficient of 0.9991. The method was applied to the analysis of river water, lake water and well water samples. The recoveries of spiked samples ranged from 81.2% to 106% with relative standard deviations between 4.5% and 7.8% (n = 6).