顶空固相微萃取-气相色谱-质谱法测定玩具中可迁移有机锡化合物  

Determination of migratory organotin compounds in toys by headspace-solid phase microextraction coupled with gas chromatography-mass spectrometry

作　　者：霍巨垣[1,2] 欧阳钢锋[2] 陈丽琼[1] 王欣[1] 

机构地区：[1]深圳市计量质量检测研究院,广东深圳518109 [2]中山大学化学与化学工程学院,广东广州510275

出　　处：《色谱》2016年第6期615-620,共6页Chinese Journal of Chromatography

基　　金：深圳市计量质量检测研究院科研基金项目(2015-YN12)~~

摘　　要：建立了顶空固相微萃取结合气相色谱-质谱联用技术测定玩具中10种可迁移有机锡化合物的方法。玩具材料经0.07 mol/L HCl浸泡2 h后,使用醋酸-醋酸钠缓冲溶液将浸泡液的pH值调至4.7,然后加入四乙基硼化钠将浸泡液中的有机锡化合物乙基化,在振荡条件下用100μm聚二甲基硅氧烷（PDMS）纤维进行顶空固相微萃取,萃取完成后将纤维插入气相色谱进样口进行热解吸,使用DB-5毛细管柱对10种有机锡化合物进行分离。10种有机锡化合物的检出限为0.5-5μg/kg。两个加标水平（0.500μg/L和5.00μg/L）下的回收率分别为80.7%-118.7%和86.2%-120.5%,RSD均低于15%。应用该方法测定了玩具可触及材料（包括涂层、织物、塑料、木料）中的可迁移有机锡化合物。该方法简便、快速、灵敏度高,不需使用有毒有机溶剂,绿色环保。A method for the determination of ten migratory organotin compounds in toys was developed using headspace-solid phase microextraction（HS-SPME）coupled with gas chromatography-mass spectrometry（GC-MS）. Toy materials were soaked in 0. 07 mol / L HCl for 2 h,then the pH of the soak solution was adjusted to 4. 7 by HAc-NaAc buffer. After ethylized with sodium tetraethylborate（NaBEt4）,the soaked solution was agitated and the headspace solid phase microextraction was performed with a 100 μm polydimethylsiloxane（PDMS）fiber. After extraction,the SPME fiber was directly injected into the GC inlet,and the organotin compounds were separated on a DB-5 capillary column. The limits of detection for the ten organotin compounds were in the range of 0. 5- 5 μg / kg. The recoveries were in the ranges of 80. 7%-118. 7% and 86. 2%- 120. 5% at the spiked levels of 0. 500 μg / L and 5. 00 μg / L. The relation standard deviations（RSDs）were all less than 15%. This method has been used to determine migratory organotin in accessible parts of toys,including coating,plastic,wood and textile.The method is simple,fast,sensitive and solvent-free.

关 键 词：顶空固相微萃取 气相色谱-质谱 有机锡化合物 玩具 

分 类 号：O658[理学—分析化学]