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

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100 μ m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0.5~5 μg/kg。两个加标水平(0.500 μg/L和5.00 μg/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。

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

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 μ m 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.