Chinese Journal of Chromatography ›› 2016, Vol. 34 ›› Issue (5): 473-480.DOI: 10.3724/SP.J.1123.2016.02018

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Simultaneous determination of 18 phenol pollutants in waste water by high performance liquid chromatography- tandem mass spectrometry

LUO Birong, WAN Xu, DENG Xingliang, YU Yuanyuan, XIE Zhenwei   

  1. Sichuan Environmental Monitoring Center, Chengdu 610091, China
  • Received:2016-02-23 Online:2016-05-08 Published:2012-12-18
  • Supported by:

    Establishment item of National Standards for Environmental Protection (No. 2014-35).

Abstract:

A method was developed for the simultaneous determination of 18 phenol pollutants in waste water by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). A volume of 5.0 mL waste water was placed into a centrifuge tube. Ammonia was added to the waste water to adjust pH≥12. A volume of 1.0 mL methylene chloride-hexane solution (2: 1, v/v) was added to the waste water, then the centrifuge tube was oscillated for 5 min and centrifuged for 5 min at 4000 r/min. The water sample was filtered through a 0.22 μ m polytetrafluoroethylene (PTFE) microfiltration membrane and adjusted to neutral by formic acid. With methanol-0.01 mol/L ammonium formate/formic acid aqueous solution (pH 4.0) as mobile phase, the separation was performed on a Thermo Hypersil ODS column (100 mm×2.1 mm, 5.0 μ m) in gradient elution. The flow rate was 0.2 mL/min. The column temperature was 30℃. The samples were detected by multiple reaction monitoring (MRM) mode with negative electrospray ionization. The phenol pollutants were quantified by external standard method. The calibration curves of the phenol pollutants showed good linearities in a suitable range with correlation coefficients (r2) not less than 0.9991. The detection limits of phenol pollutants ranged from 0.10 μ g/L to 0.88 μ g/L. The relative standard deviations of phenol pollutants were 2.5%-9.9% (n=6). The average recoveries of the 18 phenol pollutants spiked in waste water samples ranged from 68.7% to 118%(n=3). The method has been proven to be sensitive, rapid and little interference. It is suitable for the determination of the 18 phenol pollutants simultaneously in environmental waste water.

Key words: high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), phenol pollutants, waste water

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