建立了液相色谱-串联质谱法同时测定带鱼中三甲基锡(TMT)、二苯基锡(DPhT)、二丁基锡(DBT)、三苯基锡(TPhT)和三丁基锡(TBT)分析新方法。采用ZORBAX Eclipse plus C18色谱柱分离,以甲醇-甲酸/甲酸铵溶液(pH=2.15)为流动相,在流速0.3 mL·min^-1条件下,选择梯度洗脱方式分离目标物。应用液相色谱-串联质谱仪在多重反应监测(MRM)正离子模式下进行检测。有机锡化合物在选定的浓度范围内线性关系良好,相关系数均在0.994 3-0.999 8之间,三甲基锡、二苯基锡、二丁基锡、三苯基锡和三丁基锡的检测限分别为300、140、140、1和1 ng·mL^-1。方法回收率为64.7-96.9%,相对标准偏差为0.7-10.4%。
A new method was established for the simultaneous determination of trimethyltin( TMT),diphenyltin( DPhT),dibutyltin( DBT),triphenyltin( TPhT) and tributyltin( TBT) in hairtail by liquid chromatography-tandem mass spectrometry. The separation of five organotin compounds was achieved on ZORBAX Eclipse plus C18 column with gradient elution using mixture of ammonium formate solution at pH 2. 1( adjusted with formic acid) and methanol. The flow rate was 0. 3 mL / min. The detection was operated in the positive ion mode using multiple reaction monitoring. Five organotin compounds all represent good linearity in the selected concentration range,with correlation coefficients in the range of 0. 9943- 0. 9998. The detection limits of TMT,DPhT,DBT,TPhT and TBT were 300,140,140,1,1 ng·mL^- 1,respectively. Under optimized conditions,the average recoveries were ranged from 64. 7% to 96. 9%,with RSDs from 0. 7% to 10. 4%,respectively.