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    在线双固相萃取-超高效液相色谱-三重四极杆串联质谱法测定水质中19种全氟化合物的残留量

    Determination of Residues of 19 Perfluoroalkyl Compounds in Water Quality by Online Dual Solid Phase Extraction-Ultra-High Performance Liquid Chromatography-Triple Quadrupole Tandem Mass Spectrometry

    • 摘要: 取10 mL经0.45 µm玻璃纤维滤膜过滤的水样,加入1 μg·L-1混合内标溶液100 µL,混合后过0.22 µm一次性聚醚砜针头过滤器,滤液中全氟化合物(PFCs)采用在线双固相萃取系统富集后进入超高效液相色谱-三重四极杆串联质谱仪,在Waters BEH C18色谱柱上以乙腈-2 mmol·L-1乙酸铵溶液体系进行梯度洗脱分离,在电喷雾离子(ESI)源负离子模式和多反应监测(MRM)模式下进行质谱分析,内标法定量。结果显示,19种PFCs的质量浓度在一定范围内和其对应的峰面积与内标峰面积的比值呈线性关系,检出限(3S/N)为0.01~0.03 ng·L-1。以地表水、地下水、饮用水和工业废水为基质进行加标回收试验,回收率为84.1%~118%,测定值的相对标准偏差(n=6)为2.2%~6.8%。

       

      Abstract: The water sample was passed through a 0.45 µm glass fiber filter membrane, and an aliquot (10 mL) was taken. Then, the 100 µL of 1 µg·L-1 mixed internal standard solution was added. After mixing well, the mixed solution was passed through a 0.22 µm disposable polyethersulfone syringe filter. Perfluoroalkyl compounds (PFCs) in the filtrate were enriched using online dual solid phase extraction system and then introduced into ultra-high performance liquid chromatograph-triple quadrupole tandem mass spectrometer. Separation was performed on Waters BEH C18 column using the gradient elution system consisting of acetonitrile and 2 mmol·L-1 ammonium acetate solution. Mass spectrometric analysis was conducted in negative ion mode of electrospary ion (ESI) source with multiple reaction monitoring (MRM) mode, and quantification was achieved using the internal standard method. It was showed that linear relationships of the mass concentrations of the 19 PFCs and ratios of their peak areas to internal standard peak areas were kept in definite ranges, with detection limits (3S/N) in the range of 0.01-0.03 ng·L-1. Spike recovery tests were performed using surface water, groundwater, drinking water, and industrial wastewater as matrices, giving recoveries in the range of 84.1%-118%, and RSDs (n=6) of the determined values ranged from 2.2% to 6.8%.

       

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