衍生化气相色谱–质谱法测定玩具涂层中可迁移有机锡  

Determination of transportable organotin compounds in coating on toys by derivatization and gas chromatography-mass spectrometry

作　　者：孙玉慧[1] 蒋小良[1] 曾铭 王斌[3] 李达光[1] 易碧华 

机构地区：[1]江门出入境检验检疫局,广东江门529000 [2]花都出入境检验检疫局,广东广州510800 [3]东莞出入境检验检疫局,广东东莞523000

出　　处：《电镀与涂饰》2016年第6期320-324,共5页Electroplating & Finishing

基　　金：国家质量监督检验检疫总局科技计划项目(2015IK074);广东检验检疫局科技计划项目(2015GDK54);江门市科技计划项目(201501003001318)

摘　　要：建立了气相色谱-质谱法测定玩具涂层中可迁移有机锡化合物[OTs,包括二甲基锡（DMT）、一丁基锡（MBT）、二丁基锡（DBT）、四丁基锡（Te BT）、二苯基锡（DPh T）和二辛基锡（DOT）]含量的分析方法。样品用0.07 mol/L盐酸溶液浸泡提取其中的可迁移有机锡,经四乙基硼酸钠衍生化后,再进行气相色谱-质谱选择离子方式（SIM）测定。对衍生化时间和衍生化试剂用量进行了优化。在质量分数为2%的四乙基硼酸钠溶液用量为2.0 m L,衍生化时间为25 min的条件下,方法的线性相关系数均大于0.999,最低检出限达到0.01 mg/kg。在0.2 mg/L和1.0 mg/L加标水平下,加标回收率分别为83.2%～92.3%和92.6%～98.9%,相对标准偏差小于3.8%,满足欧盟玩具安全新指令2009/48/EC的检测要求。A method for the determination of transportable organotin compounds（OTs） including dimethyltin（DMT）, n-butyltin（MBT）, dibutyltin（DBT）, tetrabutyltin（Te BT）, diphenyltin（DPh T）, and dioctyltin（DOT）] in coatings on toys by gas chromatography-mass spectrometry（GC-MS） was developed. Trace amount of the transportable organotin compounds in samples are extracted by immersing in 0.07 mol/L hydrochloric acid, derivatized by sodium tetraethylborate, and then detected by GC-MS in selective ion mode（SIM）. The derivatization time and dosage of derivatization reagent were optimized. Under the conditions of sodium tetraethylborate solution（2wt%） dosage 2.0 m L and derivatization time 25 min, the linear correlation coefficients are all over 0.999, with a lowest detection limit of 0.01 mg/kg. The recoveries of OTs range from 83.2% to 92.3% and from 92.6% to 98.9% for the spiked levels 0.2 and 1.0 mg/L respectively, with a relative standard deviations lower than 3.8%, meeting the determination requirements of Directive 2009/48/EC of the European parliament and of the council of 18 June 2009 on the safety of toys.

关 键 词：玩具涂层 有机锡化合物 衍生化 气相色谱-质谱法 盐酸提取 

分 类 号：O657[理学—分析化学] O614.4[理学—化学]