正交实验优化顶空气相色谱-质谱法快速筛查玩具中致敏性芳香剂  

Study on orthogonal optimization for fast screening of allergenic fragrance in toys by headspace-Gas chromatography-Mass spectrometry

作　　者：林志惠[1] 陈丽琼[1] 幸苑娜[1] 叶雨萌 颜伟贤 陈泽勇[1] 

机构地区：[1]深圳市计量质量检测研究院,深圳518109 [2]赛默飞世尔科技(中国)有限公司,上海510030

出　　处：《分析试验室》2017年第9期1036-1041,共6页Chinese Journal of Analysis Laboratory

基　　金：国家质量监督检验检疫总局科技计划项目(2015QK171)资助

摘　　要：采用顶空气相色谱-质谱联仪(HS-GC-MS)建立起一种聚合物材料玩具中同时测定20种芳香剂的快速筛查分析方法。研究了顶空平衡温度、平衡时间以及加压压力等3种因素对20种致敏性芳香剂响应值(峰面积)的影响,并在此基础上利用正交实验,得出顶空进样的最优操作条件为:平衡温度180℃,平衡时间50 min,加压压力100 k Pa。聚合物材质的玩具样品经剪刀剪碎至5 mm×5 mm以下后,称取1 g后,并放置于密闭的容器中,在最优操作条件下直接采用顶空进样,经GC-MS进行定性及定量分析。结果表明,20种目标分析物在范围为10~400 mg/kg内呈现较好的相关性,其相关系数(r^2)均大于0.99,其方法定量限(LOQs)为0.035~4.2 mg/kg。此外,本研究通过采用回收率校正方式,建立起HS-GC-M S测得的挥发量与总量之间的关系,并利用此校正方式,实现挥发量对玩具样品中20种致敏性芳香剂总量的预测。将本文所建立的方法应用于实际玩具样品的分析,预测值能有效地避免假阴性结果的出现,其结果满足欧盟玩具安全指令2009/48/EC的检测要求。In this paper,a method of headspace-gas chromatography-mass spectrometry（ HS-GC-MS）was developed for simultaneously rapid screening of 20 fragrance allergens in polymer material toys.The effect of 20 fragrance allergens responses on different operating parameters such as equilibrium temperature,equilibrium time and pressurization were investigated. The optimal condition of head sampling resulted from orthogonal experiment was as follows： 180℃ as equilibrium temperature,50 min as equilibrium time and 100 k Pa as pressurization. The polymer material toys were crushed into side under 5 mm × 5 mm,put into close container,and subjected to headspace sampling at the optimal condition,and determined qualitatively and quantitatively by GC-MS. The method showed a good linearity in the range of 10 - 400 mg/kg with correlation coefficients（ r^2） more than 0. 99,and the limits of quantification（ LOQs） for 20 target analytes ranging from 0. 035 mg/kg to 4. 2 mg/kg. In addition,the correlation of recovery was introduced to establish relationship between the volatilization amount detected by HS-GC-MS and the total amount. The amount of 20 fragrance allergens could be predicted by volatilization amount using the correlation of recovery. This method has been applied toactual toys,and the result showed that this method could effectively avoid the false-negative results.

关 键 词：快速筛查 顶空进样 致敏性芳香剂 玩具 正交实验 

分 类 号：TQ320.77[化学工程—合成树脂塑料工业]