摘要
采用高效液相色谱串联电喷雾质谱法(LC-ESI-MS)测定纺织品中六溴环十二烷(HBCD)的含量。样品经二氯甲烷索氏提取和浓硫酸净化后,浓缩的残留物用乙腈定容,以甲醇、乙腈和乙酸铵为流动相,经反相色谱柱分离后,用电喷雾质谱在选择离子模式下(SIM)检测α,β和γ-HBCD异构体。定量离子为m/z641,定性离子为m/z637,639,643和645。α,β和γ-HBCD的定量限(S/N=10)为1.0,0.5和1.0 mg/kg,回收率在75.7%～119%,RSD值在2.35%～8.05%。
High performance liquid chromatography-electrospray ionization-mass spectrometry was applied to determine the hexabromocyclododecan （HBCD） in textiles. Samples were extracted with dichloromethane and purified with concentrated sulfuric acid. The residual was dissolved in acetonitrile, and then separated by reversed phase liquid chromatography with methanol, acetontrile and ammonium acetate as a mobile phase, α,β and γ-HBCD isomers were detected by electrospray ionizationmass spectrometry in setective ion monitoring （SIM） mode with m/z 645 as quantitative ion and m/z 637,639,641 and 643 as a qualitative ions. Limits of quantification of α,β and γ-HBCD were 1.0, 0.5 and 1.0 mg/kg separately, recoveries were 75. 7% - 119% and RSD value were 2.35% -8.05%.
出处
《印染》
北大核心
2010年第9期36-39,共4页
China Dyeing and Finishing
基金
质检公益性行业科研专项项目"纺织品化学残留释放评估
快速检测及替代品技术研究"
项目编号:200910013
关键词
测试
液相色谱
电喷雾质谱
六溴环十二烷
纺织品
testing
liquid phase chromatography
electron spray mass spectrometry
hexabromocyclododecane
textiles
作者简介
丁友超（1977-），男，工程师，从事生态纺织品检测研究。
