Journal of Korean Society on Water Environment (한국물환경학회지)

Korean Society on Water Environment (한국물환경학회)
권호 표지

Fast and Accurate Determination of Algal Toxins in Water using Online Preconcentration and UPLC-Orbitrap Mass Spectrometry

온라인 시료주입과 UPLC-Orbitrap 질량분석법을 이용한 수질 조류독소의 고속분석방법 개발 및 환경시료적용

  • 장제헌 (한국수자원공사 수질분석연구센터) ;
  • 김윤석 (한국수자원공사 수질분석연구센터) ;
  • 최재원 (한국수자원공사 수질분석연구센터)
  • Published : 2012.11.30
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Abstract

Due to the fast response to algae bloom issue in drinking water treatment plant, very fast determination methodology for algal toxin is required. In this study, column switching technique based online preconcentration method was combined with high resolution full scan mass spectrometer to save sample preparation time and to obtain fast and accurate result. After parameter optimization of online preconcentration, 1mL filtered sample was directly injected to trap column with switching valve system. Next, target toxins are eluted by 98% acetonitrile and analysed with 150 - 1,100 amu scan range at 50,000 resolving power. Method detection limit (MDL) for microcystin-LR, the most toxic isomer, was 0.1 ng/mL and others such as microcystin-YR, microcystin-RR and nodularin were 0.08, 0.03 and 0.04 ng/mL, respectively. This is the best improved sensitivities with 1mL volume in the literature. Furthermore, due to the use of ultra pressure HPLC (UPLC), the whole method run was completed in 4 min. Real sample applications for 173 sample including 55 surface water and 118 treatment plant samples for raw and treated water could be done within 16 hours. In our calculation, this methodology is roughly 80% faster than the previous manual solid-phase extraction with LC-MS/MS method.

Keywords

References

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