HPLC-ICP-MS联用技术测定玩具中痕量可迁移有机锡

王欣; 幸苑娜; 陈泽勇; 林浩学

doi:10.7538/zpxb.2013.34.02.0115

HPLC-ICP-MS联用技术测定玩具中痕量可迁移有机锡

Determination of Trace Migratory Organo-Tin in Toys by HPLC-ICP-MS

摘要

摘要: 建立了高效液相色谱-电感耦合等离子体质谱 (HPLC-ICP-MS) 联用技术测定玩具中痕量可迁移有机锡的方法。采用Waters Acquity UPLC HSS T3分析柱，在流动相为V（乙腈）∶V(水)∶V (乙酸)=65∶23∶12的混合溶液中加入0.1%三乙胺作为离子对试剂，在pH 3.0条件下，可以很好地分离二丁基锡（DBT）、三苯基锡（TPhT）、三丁基锡（TBT）和二辛基锡（DOT）。此方法简便、快速、灵敏度高，在50 μL进样量下，DBT、TPhT、TBT及DOT的检出限分别为0.08、0.24、0.14和0.65 μg/L；在5、50 μg/L两个加标水平下，回收率分别为80.7%~96.3%和83.5%~100.4%，方法精密度优于4.7%，可以满足测定要求。应用该方法测定了玩具可接触部分材料，包括织物、木料、塑料、涂层中的可迁移有机锡，分析结果令人满意。

Abstract: A method for determinating trace migratory organo-tin in toys by high performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICP-MS) was developed. The organo-tin species dibutyltin(DBT), triphenyltin(TPhT), tributyltin(TBT) and dioctyltin(DOT) were separated on Waters Acquity UPLC HSS T3 analysis column using the mobile phase of V (acetonitrile)∶V (water)∶V (acetic acid)=65∶23∶12，0.1% triethylamine with pH 3.0. This method is quickly and high sensitivity. The detection limits are 0.08, 0.24, 0.14 and 0.65 μg/L for DBT, TPhT, TBT and DOT with injection volume of 50 μL. The recoveries are 80.7%—96.3% and 83.5%—100.4% for the spiked levels of 5 and 50 μg/L, and the RSDs are less than 4.7%, which meet the determination requirements. This method has been used to determine migratory organo-tin in accessible parts of toys, including coating, plastic, wood and textile.

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