Chinese Journal of Chromatography

Chinese Journal of Chromatography

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Determination of Trace Microcystins in Water by Ultra Performance Liquid Chromatography/Tandem Mass
Spectrometry

WANG Jing1, PANG Xiaolu1, LIU Zhengzheng2, HOU Jingde3

  

  1. 1.Zhejiang Province Environmental Monitoring Centre, Hangzhou 310012, China;
    2.Department of Chemistry, Zhejiang University, Hangzhou 310027, China;
    3.Center of Analysis &Measurement, Zhejiang University, Hangzhou 310027, China

  • Received:2005-09-22 Revised:2005-12-01 Online:2006-07-30 Published:1986-12-25
  • Contact: WANG Jing

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Abstract:

An analytical method for the analysis of trace microcystins (MCYST) in water was developed
using solid phase extraction (SPE) for enrichment and ultra performance liquid chromatography/tandem
mass spectrometry (UPLC/MS/MS) for detection. One litre of water was passed through SPE columns,
the extracted sample was rinsed off by 10 mL methanol, then evaporated to 1.0 mL before being
analyzed with UPLC/MS/MS. The effect of formic acid concentration in the mobile phase on the
sensitivity was studied and the results showed that 0.1% was the optimum concentration. Four
microcystins, MCYST-LR, RR, LW, LF, can be separated and detected in 5 min, which is much shorter
than that by the conventional liquid chromatography. The detection limits were 1.3-6.0 ng/L, and the
recoveries were 91.1%-111%. The calibration curves showed good linearity in the range of 1.0
μg/L-1.0 mg/L with correlation coefficients larger than 0.99. The method was also applied to
determine MCYST in real water samples from three reservoirs in Zhejiang Province, and the results
showed that the concentrations of LR and RR were 0.0447-2.73 μg/L and 0.0208-1.36 μg/L
respectively, and LW and LF were not detected.

Key words:
multiple reaction monitoring, tandem mass spectrometry (MS/MS), microcystin, water , ultra performance liquid chromatography （UPLC）