液相色谱-串联质谱法测定食品接触材料中的六溴环十二烷  

Determination of Hexabromocyclododecane in Food Contact Materials by Liquid Chromatography Tandem Mass Spectrometry

作　　者：马强[1] 李文涛[1] 孙慧媛[1] 于红梅[1] 李晶瑞[1] 孟宪双[1] 白桦[1] 王星[1] 王超[1] 

机构地区：[1]中国检验检疫科学研究院,北京100123

出　　处：《分析测试学报》2013年第1期133-137,共5页Journal of Instrumental Analysis

基　　金：国家认证认可监督管理委员会计划资助项目(2010B161);国家质量监督检验检疫总局科技计划项目(2011IK285);中国检验检疫科学研究院基本科研业务费专项资金资助项目(2012JK020)

摘　　要：建立了同时测定高分子材料类食品接触材料中α,β,γ-六溴环十二烷的液相色谱-串联质谱分析方法。食品接触材料样品以丙酮为溶剂超声提取,提取液经ENVI-CarbⅡ/PSA固相萃取柱净化,收集二氯甲烷-正己烷(2∶3)洗脱液,采用Waters XBridge C18色谱柱(150 mm×2.1 mm,3.5μm),以甲醇-乙腈-水(41∶41∶18)为流动相等度洗脱分离后进行LC-MS/MS多反应监测模式下的定性及定量分析。α,β,γ-六溴环十二烷的方法定量下限均为40μg/kg,在40.0～160.0μg/kg范围内的低、中、高3个加标水平的平均回收率为86%～91%,相对标准偏差为1.9%～4.7%。该方法准确、快速、灵敏,可应用于食品接触材料的实际检验工作。A comprehensive analytical method based on liquid chromatography -tandem mass spec- trometry was developed for the determination of a, β, γ-hexabromocyclododecane in polymer food contact materials. The samples were ultrasonically extracted with acetone as extraction solvent. The extract was cleaned up with ENVI -Carb 11/PSA solid phase extraction cartridge. The separation of the analyte was performed on a Waters XBridge Cis （ 150 mm x 2. 1 mm, 3.5 μm） column using methanol- acetonitrile- water（41 ： 41 ： 18） as mobile phase by isobaric elution. The qualitative and quantitative analysis of the analyte were carried out under the multiple reaction monitoring （MRM） mode. The limits of quantitation （LOQs） for a, β, γ-hexabromoeyclododecane were all 40 μg/kg. The mean recoveries at three spiked levels of 40. 0 - 160. 0 μg/kg were in the range of 86% -91% , with relative standard deviations （RSDs） of 1.9% - 4.7% . The method was accurate, rapid and sensitive and was applicable to the inspection of hexabromocyclododecane in food contact materials.

关 键 词：食品接触材料 六溴环十二烷 液相色谱-串联质谱 

分 类 号：O657.63[理学—分析化学] TQ314.248[理学—化学]