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 chroma-tography-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 com-pounds 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.
参考文献
| [1] | Tutschku S.;Schantz MM.;Wise SA..Determination of methylmercury and butyltin compounds in marine biota and sediments using microwave-assisted acid extraction, solid-phase microextraction, and gas chromatography with microwave-induced plasma atomic emission spectrometric detection[J].Analytical chemistry,200218(18):4694-4701. |
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