ASE-LC-MS/MS技术检测水产品中六溴环十二烷

Determination of HBCDS in Aquatic Product by ASE-LC-MS/MS

建立了快速溶剂萃取-超快速液相色谱-串联质谱（ASE-LC-MS/MS）测定水产品中六溴环十二烷（HBCDS）的方法。试样经冷冻粉碎后,以V（丙酮）∶V（正己烷）=1∶1的溶液为萃取液,采用快速溶剂萃取法,以水-甲醇为流动相,经C_（18）柱分离后,以快速液相色谱-串联质谱法多反应监测扫描模式进行定性和定量分析。结果表明,最低检出限为2μg/L,加标回收率为89%-104%,相对标准偏差小于15%;在10-200μg/L,线性范围内线性关系良好,相关系数均大于0.998。该方法灵敏度高、重现性好、定性定量准确,适用水产品的复杂基质样品检测,可为相关国家标准制定提供参考依据。

Establish an accelerated solovent extraction-ultra performance liquid chromatography-tandem mass spectrometry （ASE-LC-MS/MS） method for HBCDS in aquatic product. V （Acetone） ： V（Hexane）=1： 1 as an extraction solvent was been adopted. The brominated flame retardants residue was separated by HPLC using methanol-water as the mobile phase, and was detective using electrospray ionization （ESI） on a tandem mass spectrometer in multiple reactions monitoring mode. The results showed that low detection limit was 2 μg/L, and the average recoveries of HBCDS were 89%-104%, relative standard deviations were less than 15%. The HBCDS behaved linearly in the wide range of 10-200 μg/L with the correlation coefficients more than 0.998. This method was sensisitive, recurrent and accurate. It could be used for aquatic product and provide reference for the relevant national standards setting.