微波消解-电感耦合等离子体质谱法筛选玩具材料中11种有机锡  

Rapid Screening of 11 Organotins in Toy Materials by Microwave Assisted Digestion-Inductively Coupled Plasma Mass Spectrometry

作　　者：田勇[1] 丁志勇[1] 刘崇华[1] 黄理纳[1] 

机构地区：[1]广东检验检疫技术中心,广东广州510623

出　　处：《化学试剂》2016年第5期447-450,共4页Chemical Reagents

基　　金：广东省科技计划项目(503243100055);广东出入境检验检疫局科技项目(2014GDK18)

摘　　要：提出了无机锡标准曲线法测定有机锡的假阳性和假阴性问题，建立了测试总量锡筛选有机锡的方法。以6mL硝酸加2mL盐酸为酸体系，采用微波消解仪前处理样品，用电感耦合等离子体质谱法（ICP-MS）筛选玩具材料中禁限用的有机锡。选取易出现有机锡超标的高风险材料油漆涂层、ABS塑料、PP塑料、PVC塑料、皮革等作为典型玩具样品，进行加标及阳性样品验证。11种有机锡加标以元素锡计的回收率为87．0％～109．6％，加标测试相对标准偏差（RSD）〈4．8％，实际阳性样品测试RSD〈6．4％，具有良好的准确度和精密度。建立的方法以元素锡计的定量限为0．14mg／kg，可实现欧盟玩具安全新指令涉及的第三类玩具材料中有机锡的快速筛选目标。Pointing out the phenomenon that false positives and false negatives may appeared when determinating of organotin by standard curve method with inorganic tin. The toy samples are pretreated by microwave digestion with 6 mL of nitric acid and 2 mL of hydrochloric acid,and limited organotins are then screened by inductively coupled plasma-mass spectrometer （ICP-MS）. Materials of high risk, especially those with potential high possibility exceeding migration limit of organotins, including paint coatings, ABS plastics,polypropylene plastlcs,polyvinylchloride plastics,leather etc, are selected to conduct standard addition experiments and positive sample validation. Recoveries of tin are between 87.0% to 109.6% ,and RSD is less than 4. 8%. Moreover,RSD is less than 6.4% when screening positive samples,indicating satisfactory accuracy and precision of this method. LOQ of this method is 0. 14 mg/kg on the basis of tin,which makes it feasible to rapidly screen organotins of all categories m of toy materials specified in EU toy safety directive.

关 键 词：玩具 有机锡 微波消解 电感耦合等离子体质谱仪 

分 类 号：O657.6[理学—分析化学] O614.432[理学—化学]