分析测试学报2018，Vol.37Issue(6)：714-718,5.DOI:10.3969/j.issn.1004-4957.2018.06.012
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
摘要
Abstract
A method was developed for the determination of hexabromocyclododecanes (HBCDs) in marine organisms by high performance liquid chromatography ― tandem mass spectrometry (H PLC-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 elu-ting 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 0.20μg/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)Key words
solid phase extraction (SPE)/UPLC-MS/MS/marine organisms/hexabromocyclododecanes (HBCDs)分类
化学化工引用本文复制引用
严忠雍,张小军,陈雪昌,方益,张帅,孙秀梅..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[J].分析测试学报,2018,37(6):714-718,5.基金项目
国家自然科学基金资助项目(21407127) （21407127）
浙江省科技计划项目(2017C37009) （2017C37009）
