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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。
A rapid solvent extraction-ultra-fast liquid chromatography-tandem mass spectrometry (ASE-LC-MS / MS) was developed for the determination of HBCDS in aquatic products. After the sample was frozen and crushed, the solution was extracted with V (acetone): V (n-hexane) = 1: 1 by using the rapid solvent extraction method and the mobile phase consisted of water and methanol. , Qualitative and quantitative analysis was performed with a rapid liquid chromatography-tandem mass spectrometry multi-reaction monitoring scan mode. The results showed that the minimum detectable limit was 2μg / L, the spiked recoveries were 89% -104% and the relative standard deviations were less than 15%. The linearity was good in the range of 10 ~ 200μg / L with the correlation coefficients above 0.998. The method has the advantages of high sensitivity, good reproducibility, qualitative and quantitative accuracy, and detection of complex matrix samples suitable for aquatic products, which can provide reference for the formulation of relevant national standards.