HPLC-MS法分析海洋沉积物中的全氟化合物

Determination and application of PFCs in sediment by HPLC-MS/MS

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 was developed for the 17 perfluorinated compound（ PFCs） in sediment by high performance liquid chromatography-tandem mass spectrometry（ HPLC-MS/MS）. The sample was extracted with the mixed liquids of Na OH and CH3 OH concentrated and cleaned up by a HLB solid phase extraction column. The extracting solution was eluted by CH3 OH and dried with N2 and concentrated with 1 m L CH3 OH. The 17 PFCs were separated by a C18 column（ 150 mm × 2. 1 mm,3. 5 μm） and confirmed by MS/MS under multiple reaction monitoring（ MRM） mode and quantified by internal standard method. The calibration curves of 17 PFCs were liner in the concentration range of 0. 5 ~ 50 ng/m L with correlation coefficients（ r） of 0. 9902 ~ 0. 9988 under the optimum conditions. The limits of detection（ S/N = 3） ranged from 0. 03 to 0. 05 ng/g. The mean recoveries of 17 PFCs at spiked levels of 5. 0,10,20 ng were in the range of 71. 0% ~ 115. 7% with relative standard deviation（ n = 3） of 0. 39% ~ 6. 4%. The method was applied to determination of PFCs in sediment from Laizhou Bay. 17 PFCs were all detected in all sediment.