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液-液微萃取-HPLC-ICP-MS联用技术测定玩具中痕量可迁移六价铬 被引量:4

Determination of Trace Transportble Hexavalent Chrome in Toys by DLLME-HPLC-ICP-MS Method
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摘要 基于玩具样品水迁移相中的六价铬首先与吡咯烷二硫代氨基甲酸铵络合形成有机化合物,再以三氯甲烷为萃取剂、丙酮为分散剂,建立了分散液-液微萃取(DLLME)结合液相色谱-电感耦合等离子体质谱测定六价铬的方法,同时对影响DLLME萃取效率的因素进行了优化实验。实验表明:该方法线性范围为1×10^(-8)~1×10^(-7) g/L,线性相关系数为0.9998,检出限为0.010μg/L,平均回收率范围85%~100%,方法适用于EN 71-3中II类玩具材料六价铬的检测。 A new method, dispersive liquid-liquid micro-extraction(DLLME) and high performance liq- uid chromatography (HPLC)-inductively coupled plasma mass spectrometry (ICP-MS) has been established for the determination of hexavalent chrome in aqueous solution from toy products. In this method, Hexavalent chrome in aqueous are complexed with l-pyrrolidinecarbodithioic acid firstly, and then extracted by dispersive liquid-liquid micro-extraction with methenyl trichlorid as an extraction solvent and acetone as a dispersing solvent. The experimental parameters exerting influence on extraction recoveries of hexavalent chrome by DLLME are optimized. The results show that the linearity range of this method is 1×10^-8-1×10^-7 g/L the linearity correlation coefficient is 0.9998, the method detection limit is 0.010μg/L and the average recovery rate is 85%-100%. This method is suitable for the determination of hexavalent chrome in category Ⅱ toy material defined in EN 71-3.
出处 《浙江化工》 CAS 2016年第6期37-42,共6页 Zhejiang Chemical Industry
基金 浙江省科技计划项目(2014C37060)
关键词 分散液-液微萃取 HPLC-ICP-MS 六价铬 dispersive liquid-liquid micro-extraction(DLLME), HPLC-ICP-MS, hexavalent chrome
作者简介 邹学权(1976-),男,江苏徐州人,博士,工程师。主要从事进出口工业消费品及食品的检验检测。E-mail:zouxq@ziq.gov.cn。
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