온라인 시료주입과 UPLC-Orbitrap 질량분석법을 이용한 수질 조류독소의 고속분석방법 개발 및 환경시료적용 |
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학술지명 한국물환경학회
저자 장제헌,김윤석,최재원
발표일 2012-07-17
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Cyanobacterial blooms can form in warm, slow-moving waters that are rich in nutrients. Typical algal blooms often occur in late summer or early fall. But now, fast response to analysis of algal toxin is needed considering global scaled climate change and the latest unexpected algal blooming in upstream of metropolitan watershed. In this study, column switching technique based online preconcentration was combined with high resolution full scan mass spectrometer to save sample preparation time and to obtain accurate result. After optimization of this methodology, 1mL filtered sample was directly injected to preconcentration column without further process. Next, target toxins are detected with 150 - 1,100 amu scan range at 50,000 resolving power. Method detection limit 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 in the literature. Furthermore, due to the use of 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 two days. In our calculation, this methodology is 92% faster than the previous manual solid-phase extraction with LC-MS/MS method. |