超临界二氧化碳流体萃取法测定玩具中15种致敏芳香化合物  

Determination of 15 Fragrance Allergens in Toys by Supercritical Carbon Dioxide Fluid Extraction

作　　者：郑琳[1] 林力[1] 曹国洲[1] 王谦[1] 金献忠[1] 卫碧文[2] 曹良惠[1] 

机构地区：[1]宁波出入境检验检疫局,浙江宁波315012 [2]上海出入境检验检疫局,上海200135

出　　处：《分析测试学报》2014年第1期51-56,共6页Journal of Instrumental Analysis

基　　金：宁波市自然科学基金项目(2011A610083)

摘　　要：该文以欧盟新玩具指令中限用或禁用的15种致敏芳香化合物为研究目标,研究了超临界二氧化碳萃取压力、温度、夹带剂等条件对萃取效率的影响,建立了超临界流体萃取/气相色谱-质谱联用仪测定玩具中15种致敏芳香化合物的分析方法.最佳萃取条件为：萃取温度50℃,压力300 bar,二氧化碳流速30g/min,夹带剂甲醇含量3％,动态萃取30 min,静态萃取30 min.萃取物经DB-17MS色谱柱分离后,采用质谱仪进行检测,内标法定量.15种化合物在0.02～60 μg/mL范围呈良好线性,相关系数为0.993 2～0.9999,检出限（S/N=10）为0.02～0.09 μg/mL.该法检测聚丙烯（PP）、聚乙烯（PE）、丙烯腈-丁二烯-苯乙烯（ABS）塑料的回收率分别为79.6％～114.5％、75.0％～118.9％、72.7％～114.9％,相对标准偏差为3.2％～11.0％、0.6％～11.6％、3.5％～11.0％.建立的方法灵敏、环保,可用于玩具中致敏芳香化合物的检测.A method of supercritical CO2 fluid extraction gas chromatography-mass spectrometry （GC-MS） was developed for the determination of fragrance allergens in toy material.The optimal conditions were as follows：extraction temperature：50 ℃,pressure：300 bar; carbon dioxide flow rate：30 g/min; content of methanol entrainer：3％,dynamic extraction：30 min; static extraction time：30 min.Under the optimal conditions,the extracts were separated on a DB-17MS column,then determined by GC-MS and quantified by the internal standard method.The calibration curves were linear in the range of 0.02-60 μg/mL with correlation coefficients of 0.993 2-0.999 9 and detection limits（S/N =10） of 0.02-0.09 μg/mL.The average recoveries of the target compounds in polypropylene （PP）,polyethylene （PE）,alkyl benzo sulfonate （ABS） plastic samples were in the ranges of 79.6％-114.5％,75.0％-118.9％ and 72.7％-114.9％,respectively.The relative standard deviations were in the ranges of 3.2％-11.0％,0.6％-11.6％,3.5％-11.0％.The results showed that this method was sensitive,reliable and environmental for the qualitative and quantitative determinations of fragrance allergens in toy product.

关 键 词：超临界二氧化碳流体萃取 气质联用仪 致敏芳香化合物 玩具 

分 类 号：O657.63[理学—分析化学] O625[理学—化学]