建立了海洋沉积物中17种全氟化合物的高效液相色谱-串联质谱分析方法。采用Na OH-甲醇提取样品,并用HLB固相萃取柱对样品进行富集净化,然后用甲醇进行洗脱,洗脱液氮气浓缩,甲醇定容后,采用Waters SymmetryC18色谱柱(150 mm×2.1 mm,3.5μm)分离,电喷雾负离子多反应监测(MRM)模式检测。在最佳实验条件下,17种化合物的体积分数在0.1~50 ng/m L范围内呈线性(r>0.9902),加标回收率在67.37%~111.4%之间,相对标准偏差为0.39%~6.4%,检出限为0.03~0.05 ng/g。将方法应用于莱州湾海洋沉积物中目标物的检测,11个站位点中17种化合物均有检出。 A method for the determination of 17 perfluorinated compounds in marine sediment by high performance liquid chromatography-tandem mass spectrometry was established. The sample was extracted with NaOH-methanol, and the sample was concentrated and purified by HLB SPE. The sample was then eluted with methanol. The eluate was concentrated under nitrogen. After the methanol was denatured, the residue was purified by a Waters Symmetry C18 column (150 mm × 2.1 mm , 3.5μm) separation, electrospray negative ion multiple reaction monitoring (MRM) mode detection. Under the optimal experimental conditions, the volume fraction of 17 compounds was linear (r> 0.9902) in the range of 0.1 ~ 50 ng / m L with the recoveries of 67.37% ~ 111.4% and the relative standard deviations of 0.39% ~ 6.4%, the detection limit was 0.03 ~ 0.05 ng / g. The method was applied to the detection of targets in marine sediments in Laizhou Bay, and 17 compounds were detected in 11 stations.