Journal of Korean Society on Water Environment (한국물환경학회지)

Korean Society on Water Environment (한국물환경학회)
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Evaluation of Pre-treatment Stages for Microcystins Analysis using LC/MS/MS

LC/MS/MS 분석을 위한 microcystins 전처리 단계별 효율성 연구

  • Kim, Hwa-Bin (Han River Water Environment Research Center, National Institute of Environmental Research) ;
  • Park, Hae-Kyung (Han River Water Environment Research Center, National Institute of Environmental Research) ;
  • Moon, Jeong-Suk (Han River Water Environment Research Center, National Institute of Environmental Research)
  • 김화빈 (국립환경과학원 한강물환경연구소) ;
  • 박혜경 (국립환경과학원 한강물환경연구소) ;
  • 문정숙 (국립환경과학원 한강물환경연구소)
  • Received : 2009.06.01
  • Accepted : 2009.07.28
  • Published : 2009.09.30
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Abstract

We investigated the most effective pre-treatment processes and LC/MS/MS condition for microcystins analysis. With a step-by-step pre-treatment, efficiencies of several established methods were compared. At the level of cell burst, sonication method was found to be the most efficient. As a mycrocystins first extraction solvent, 5% acetic acid showed the highest efficiency. An isolation and recovery rate of mycrocystins of ODS Sep-Pak $C_{18}$ cartridge was higher than HLB SPE cartridge. As a final elution solvent from cartridge, 100% MeOH had a better efficiency than others. Using a LC/MS/MS, effective analytical methods were established. C18 reverse column was used and gradient elution was performed with using acetonitrile, 0.1% formic acid as a mobile phase. We analysed to 0.8 mL/min flow rate fit to the $5{\mu}m$ particle size column and $55^{\circ}C$ housing temperature. The validity of established analytical method was evaluated that MDL as average $0.050{\pm}0.014{\mu}g/L$ and LOQ as average $0.160{\pm}0.045{\mu}g/L$ had a good sensitivity over 40 magnification rather than $2{\mu}g/L$ detection limit of HPLC.

Keywords

Acknowledgement

Grant : 조류예보제 발령기준 적정화 방안연구(I)

Supported by : 국립환경과학원

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