论文部分内容阅读
本文建立了运用液质联用技术,分析鱼油中的PBDE-100、PBDE-154、PBDE-047、PBDE-099、PBDE-153、PBDE-209和PBDE-028这7种多溴联苯醚残留。样品制备后经正己烷提取,经硅胶SPE小柱净化后,以C18柱为液相分离柱,以甲醇和水溶液为流动相梯度洗脱,多反应监测模式(MRM)测定,外标法定量。多溴联苯醚(PBDEs)含量在1~1 000mg/L具有良好的线性关系,检测下限为1ng/m L。以空白鱼油为基体,加入3种不同浓度水平的多溴联苯醚做加标回收试验,回收率70%~100%,相对标准偏差小于10%。该方法操作简单,结果准确,重现性好。
In this paper, we established a method for the determination of 7 polybrominated diphenyl ethers (PBDEs) in fish oil using the liquid chromatography-mass spectrometry (LC-MS / MS) technique, including PBDE-100, PBDE-154, PBDE-047, PBDE-099, PBDE-153, PBDE-209 and PBDE-028. After the sample was prepared, it was extracted with n-hexane, purified on a silica gel SPE cartridge, and separated on a C18 column. The mobile phase consisted of methanol and aqueous solution. Multiple reaction monitoring (MRM) and external standard were used. Polybrominated diphenyl ethers (PBDEs) content of 1 ~ 1 000mg / L has a good linear relationship, the detection limit of 1ng / m L. With blank fish oil as substrate, three different concentrations of PBDEs were added for spike recovery test. The recovery rate was 70% -100% and the relative standard deviation was less than 10%. The method is simple, accurate and reproducible.