超高效液相色谱-串联四极杆质谱法检测小型家电外壳中的六溴环十二烷

建立了加热回流萃取-超高效液相色谱-串联四极杆质谱检测小型家用电器中六溴环十二烷( Hexabromocyclododecane,HBCD)的方法.实验优化了电子电器类产品的前处理方法,以甲苯-甲醇(10∶1,V/V)为萃取剂,加热回流4h.萃取出的溶液经N2吹干,初始流动相复溶,涡旋、离心、过膜,经ACQUITYTMUPLC BEH C18色谱柱分离；以甲醇-乙腈(4∶1,V/V)-10 mmol/L醋酸铵为流动相,质谱的多反应监测模式(MRM)进行检测,HBCD的3种同分异构体在3 min内完全分开.该物质的检山限为0.014 mg/L:定量限为0.068 mg/L；标准曲线的线性范围为1.6～ 32.4 mg/L,线性相关系数大于0.996,萃取回收率为68.0％～75.2％.通过外标法定量,并将本方法应用于实际样品(电视机外壳、电子相框、电磁炉外壳等)的检测.

Determination of Hexabromocyclododecane in Shell of Small Household Electrical Appliances Products by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

A method for the detection of hexabromocyclododecane(HBCD) in small household electrical appliances products by heating reflux extraction-ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) was developed.After comparing the ultrasonic extraction,accelerated solvent extraction,soxhlet extraction and heating reflux extraction,the optimum pretreated method,heating reflux extraction,was selected for extracting three isomerides of HBCD in small household electrical appliances products.The mixture of toluene∶methanol=10∶1 was used as extracting solvent and heating backflow time was 4 h.The extract solution was dried by N2,and dissolved by the initial mobile phase,then vortexed,centrifuged and filtered.After the separation by BEH C18 column,the three isomerides of HBCD were detected by mass spectrometry in the negative electrospray ionization with multiple reaction monitoring(MRM) mode.The three isomerides were separated effectively in 3 min.The linear ranges of the compounds were 1.6-32.4 mg/L for HBCDs with correlation coefficient greater than 0.996.The limit of detection(LOD) and the limit of quantitation(LOQ) for HBCD were 0.014 and 0.068 mg/L,and the recoveries were 68.0%-75.2%.This method was successfully used in the analysis of real samples.