硅胶固相萃取净化/高效液相色谱-串联质谱法测定海洋生物体中六溴环十二烷  

Determination of Hexabromocyclododecanes in Marine Organisms by High Performance Liquid Chromatography-Tandem Mass Spectrometry Coupled with LC-Si SPE Clean-up

作　　者：严忠雍[1,2] 张小军 陈雪昌[1,2] 方益 张帅[1,2] 孙秀梅 YANZhong- yong;ZHANGXiao- jun;CHENXue- chang;FANGYi;ZHANGShuai;SUNXiu- mei(Marine Fisheries Research Institute of Zhejiang,Zhoushan 316021,China;Key Lab of Sustainable Utilization of Technology Research for Fishery Resource of Zhejiang,Zhoushan 316021,China)

机构地区：[1]浙江省海洋水产研究所,浙江舟山316021 [2]浙江省海洋渔业资源可持续利用技术研究重点实验室,浙江舟山316021

出　　处：《分析测试学报》2018年第6期714-718,共5页Journal of Instrumental Analysis

基　　金：国家自然科学基金资助项目(21407127);浙江省科技计划项目(2017C37009)

摘　　要：建立了海洋生物体中六溴环十二烷(HBCDs)的硅胶固相萃取净化/液相色谱-串联质谱法。样品采用正己烷提取,经硅胶固相萃取柱净化,液相色谱-串联质谱分析。根据硅胶固相萃取柱的使用特性,对洗脱条件进行优化。在ACQUITY UPLC BEH C18色谱柱上进行分离,流动相为水和甲醇乙腈(V甲醇∶V乙腈=4∶6)混合溶液,梯度洗脱。质谱采用电喷雾负离子电离,多反应监测模式,内标法定量。六溴环十二烷在0.50~100.0μg/L范围内线性关系良好,相关系数(r2)大于0.995,定量下限为0.20μg/kg,回收率为85.6%~97.3%,相对标准偏差为3.9%~8.8%。该方法基质干扰小、重复性好,适用于海洋生物中六溴环十二烷的测定。A method was developed for the determination of hexabromocyclododecanes（ HBCDs） in marine organisms by high performance liquid chromatography-tandem mass spectrometry（ HPLC-MS/MS） coupled with LC-Si SPE clean-up. The samples were extracted with n-hexane,cleaned up by LC-Si SPE,and analyzed by LC-MS/MS. The major parameters affecting LC-Si SPE eluting conditions were also investigated. The chromatographic separation was performed on an ACQUITY UPLC BEH C18 column by gradient elution with water and methanol-acetonitrile solution（ methanol ∶ acetonitrile = 4 ∶ 6） as mobile phase. The detection of analyte was carried out by electrospray mass spectrometry in negative ionization under multiple reaction monitoring mode,and the internal standard method was used for quantification. There existed good linear relationships for HBCDs in the range of 0. 50-100. 0 μg/L with correlation coefficients（ r2） more than 0. 995. The quantitation limits of the method were 0. 20 μg/kg. The recoveries for HBCDs were in the range of 85. 6%-97. 3%,with relative standard deviations of 3. 9%-8. 8%. Therefore,the method could be applied in the identification and quantitation of HBCDs in marine organisms with low matrix interference and good reproducibility.

关 键 词：固相萃取(SPE) 液相色谱-串联质谱 海洋生物体 六溴环十二烷(HBCDs) 

分 类 号：O657.63[理学—分析化学] O623.11[理学—化学]