超高效液相色谱-串联质谱法同时测定塑料玩具中四溴双酚A和六溴环十二烷  

Determination of Tetrabromobisphenol A and Hexabromocyclododecanes in Plastic Toys by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：肖亮 薛芳 丛静 刘翠珍 XIAO Liang;XUE Fang;CONG Jing;LIU Cuizhen(Weihai Inspection and Research Institute of Products Quality,Standard and Metrology,Weihai 264200;Shandong Drug and Food Vocational College,Weihai 264200)

机构地区：[1]威海市产品质量标准计量检验研究院,山东威海264200 [2]山东药品食品职业学院,山东威海264200

出　　处：《分析科学学报》2022年第1期94-98,共5页Journal of Analytical Science

基　　金：国家标准制修订项目(No.20172649-T-607);山东省质量技术监督局科技项目(No.2017KY39Z00)。

摘　　要：建立了超高效液相色谱-串联质谱法(UPLC-MS/MS)同时测定塑料玩具中四溴双酚A和六溴环十二烷含量的方法。样品经丙酮-正己烷超声提取,甲醇沉淀净化后,采用UPLC-MS/MS法,以多反应监测模式测定,外标法定量。目标物在2.0~100μg/L范围内呈现良好的线性关系,相关系数大于0.9973,检出限为0.010~0.012 mg/kg,加标回收率为81.8%~97.2%,相对标准偏差为3.8%~9.9%。该方法操作步骤简单、快速、稳定性好,适用于塑料玩具中四溴双酚A和六溴环十二烷的快速筛查、确证和定量测定。A method for the determination of tetrabromobisphenol A and hexabromocyclododecanes in plastic toys was developed by ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The samples were extracted by ultrasonic with acetone-n-hexane,then precipitated by methanol.All the samples were detected in multiple reaction monitoring(MRM)mode.The calibration curve was linear in the range of 2.0-100μg/L,and all correlation coefficients were larger than 0.9973.The limits of detection were ranged from 0.010 mg/kg to 0.012 mg/kg.The spiked recoveries of 4 compounds were in the range of 81.8%-97.2%with satisfied relative standard deviations ranging from 3.8%to 9.9%.The method was simple,rapid,reliable.It could be suitable for the rapid screening,identification and quantification of tetrabromobisphenol A and hexabromocyclododecanes in plastic toys.

关 键 词：超高效液相色谱-串联质谱法 四溴双酚A 六溴环十二烷 塑料玩具 

分 类 号：O657.63[理学—分析化学]