摘要
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。
Determination of polybrominated diphenyl ethers PBDE-100 PBDE-154, PBDE-047, PBDE-099, PBDE-153, PBDE-209 and PBDE-028 in fish oil by high performance liquid chromatography mass spectrometry. Sample was extracted with normal hexane, purified by silica gel SPE. C18 column using methyl alcohol and water solution as mobile phase with gradient elute in multiple reaction monitoring ( MRM) modes and quantitated by external standard method. Linear relationship between values of peak area and mass concentration of polybrominated diphenyl ethers was obtained in range of 1ng/mL-1000 mg/L. Lower limit detection of polybrominated diphenyl ethers was 1ng/mL. Recovery test was made by addition of standard polybrominated diphenyl ethers at 3 differert concentration levels to blank samples, values of recovery found were in range from 70%to 100%. Values of RSD (n=6) found were less than 10%. This method is simple, sensitive, accurate and repeatable.
出处
《粮油加工（电子版）》
2015年第12期41-43,46,共4页
Machinery for Cereals Oil and Food Processing Main Contents
基金
上海市科学技术委员会应用技术开发专项资金项目(2014-211)
