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Evaluation of Pre-treatment Stages for Microcystins Analysis using LC/MS/MS  

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)
Publication Information
Journal of Korean Society on Water Environment / v.25, no.5, 2009 , pp. 720-726 More about this Journal
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
Cyanobacteria; LC/MS/MS; Microcystins; Pre-treatment;
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Times Cited By KSCI : 1  (Citation Analysis)
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