建立了液相色谱-串联质谱同时测定白酒中三丁基锡(TBT)和三苯基锡(TPhT)的分析新方法。10mL酒样经氮吹浓缩至3mL,用甲醇定容到10mL,再经0.22"m有机滤膜过滤。采用ZORBAX Eclipse plus C18色谱柱分离,流动相为体积比60∶40的甲醇-0.1%甲酸溶液,流速为0.3mL/min,在正离子模式下采用多重反应监测(MRM)进行分析。两组分在3min内完全分离,该方法在1~100ng/mL浓度范围内线性关系良好,相关系数均优于0.9992,TBT和TPhT的检测限分别为0.0002ng/mL和0.003ng/mL。在5、20、50ng/mL三个添加水平下回收率在77.5%~92.3%之间,其相对标准偏差均小于10.08%。该方法灵敏度高、简便,准确可靠,可用于白酒中TBT和TPhT的同时测定,效果良好。
A simple and accurate method was developed for the determination of triphenyltin and tributyltin in wine. 10 mL wine sample was blown to 3 mL by nitrogen,then 7 mL methanol was added in the sample. Finally the mixed redissolution was filtered by 0.22 μm organic filter membrane. ZORBAX Eclipse plus C18 column was used for the separation,and the mobile phase of HPLC was methanol: H20 (0.1% HCOOH)-: 60:40. The flow rate was 0.3 mL/min. The mass spectrometer was operated in the positive ion mode using multiple reaction monitoring. The good linearities between analytical signals and analyte concentration were showed in the range of 1-100 ng/L with the correlation coefficients (R2) of 0. 9992-0. 9993. For TPhT and TBT,the detection limits were 0. 003 and 0. 0002 ng/mL,respectively. In three spiked levels,the average recoveries of TPhT and TBT ranged from 77.5% to 92.3% with relative standard derivation(RSD) less than 10.08%. The proposed method was successfully applied to the determination of TPhT and TBT in wine. The results indicate this method is rapid,accurate and can be used to detect TPhT and TBT in wine.