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    磁性聚苯乙烯-Fe3O4固相萃取-超高效液相色谱-串联质谱法测定水中双酚A

    Determination of Bisphenol A in Water by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry after Solid Phase Extraction with Magnetic Polystyrene-Fe3O4

    • 摘要: 建立了磁性聚苯乙烯-Fe3O4(HCP-Fe3O4)固相萃取联用超高效液相色谱-串联质谱(UHPLC-MS/MS)的检验方法,用于测定水中双酚A (BPA)的含量。水样经HCP-Fe3O4固相萃取,用甲醇洗脱后进样,以ACQUITY UPLC BEH C18色谱柱为分离柱,以不同体积比的甲醇和水作为流动相进行梯度洗脱;质谱分析采用电喷雾负离子(ESI-)模式电离、多反应监测(MRM)模式检测。BPA的质量浓度在1.000~1 000 μg·L-1内与其峰面积呈线性关系,方法的检出限(3S/N)为0.04 μg·L-1。加标回收率为98.4%~99.9%,测定值的相对标准偏差(n=6)为2.6%~8.2%。

       

      Abstract: A method of solid phase extraction with magnetic polystyrene-Fe3O4 (HCP-Fe3O4) combined with ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) was established, which was used to determine the content of bisphenol A (BPA) in water. After extracted by HCP-Fe3O4 and eluted by methanol, water samples were separated by ACQUITY UPLC BEH C18 column, with the mixtures of methanol and water with the different volume ratios as mobile phase for gradient elution. The electrospray ionization source of MS in negative ion (ESI-) mode was used for detection under the mode of multiple reaction monitoring (MRM). Linearity relationship between values of mass concentration of BPA and its peak area was kept in the range of 1.000-1 000 μg·L-1, with limit of detection (3S/N) of 0.04 μg·L-1. Values of the spiked recovery were found in the range of 98.4%-99.9%, and RSDs (n=6) of the measured values were found in the range of 2.6%-8.2%.

       

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