液相色谱-串联质谱法同时测定玩具中5种酚类内分泌干扰物  

Simultaneous Determination of 5 Phenolic Endocrine Disruptors in Toys by LC-MS/MS

作　　者：郭项雨[1] 李海玉[1] 吕庆[1] 张庆[1] 李丕[1] 白桦[1] 王志娟[1] 王婉[1] 

机构地区：[1]中国检验检疫科学研究院,北京100123

出　　处：《理化检验（化学分册）》2015年第12期1708-1712,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金："双打"中玩具有机类有害物质检验鉴定方法研究(2012104018-12);塑胶和木制儿童用品中典型环境激素迁移规律研究(201310057)

摘　　要：采用液相色谱-串联质谱法测定玩具中5种酚类内分泌干扰物(即双酚A、对叔辛基酚、邻正壬基酚、对正辛基酚及对正壬基酚的含量)。ABS塑料玩具样品以四氢呋喃为提取溶剂,超声辅助溶解,用甲醇沉淀塑料基质;布绒玩具样品用甲醇作为提取溶剂,超声提取。提取液采用Waters XBridge C_(18)色谱柱分离,以不同比例的甲醇和0.1%(体积分数)氨水溶液的混合液作为流动相进行梯度洗脱,洗脱液供质谱分析,质谱测定中选择电喷雾负离子源和多反应监测模式。5种化合物的质量浓度在一定范围内与峰面积呈线性关系,上述5种酚类化合物的测定下限(10S/N)分别为1.0,1.0,1.0,0.5,0.5μg·kg^(-1)。加标回收率在87.4%~105%之间,测定值的相对标准偏差(n=6)均小于9.1%。LC-MS/MS was applied to the determination of 5phenolic endocrine disruptors（i.e.bisphenol A,2-octylphenol,2-nonylphenol,4-n-octylphenol and 4-n-nonylphenol）in toys.For ABS plastic toys,the sample was ultrasonically extracted with tetrahydrofuran and then the plastic matrix was separated by precipitation with methanol.For cloth fabric toys,the sample was ultrasonically extracted with methanol,and the extract was separated on Waters XBridge C_（18） column,using a mixture of methanol and（φ）0.1% ammonia solution（mixed in various ratio）as mobile phase in the gradient elution.ESI-and MRM were adopted in MS.Linear relationships were found between values of peak areas and mass concentrations of the 5phenolic endocrine disruptors in definite ranges.The lower limits of determinaiton（10S/N）for the above mentioned phenols were 1.0,1.0,1.0,0.5,0.5μg·kg^（-1） respectively.Values of recovery obtained by standard addition method were in the range of 87.4%-105%,with RSDs（n=6）were less than 9.1%.

关 键 词：液相色谱-串联质谱法 双酚A 辛基酚 壬基酚 玩具 

分 类 号：O657.63[理学—分析化学]