• 제목/요약/키워드: Online sample preconcentration

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온라인 시료주입과 UPLC-Orbitrap 질량분석법을 이용한 수질 조류독소의 고속분석방법 개발 및 환경시료적용 (Fast and Accurate Determination of Algal Toxins in Water using Online Preconcentration and UPLC-Orbitrap Mass Spectrometry)

  • 장제헌;김윤석;최재원
    • 한국물환경학회지
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    • 제28권6호
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    • pp.843-850
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    • 2012
  • 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.

온라인 자동화 시료 전처리 및 HR Orbitrap LC/ESI-MS를 이용한 환경시료 중 잔류 의약물질 분석방법 확립 (Establishment of the Analytical Method for Residual Pharmaceuticals in Raw Water Using Online Sample Preparation and High Resolution Orbitrap LC/ESI-MS)

  • 황윤정;신상희;박종숙
    • 한국물환경학회지
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    • 제29권3호
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    • pp.409-419
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    • 2013
  • In this study, the analytical method for 27 residual pharmaceuticals in raw water was developed. Online sample preconcentration/extraction and analysis with high resolution Orbitrap mass spectrometry (LC-ESI/Orbitrap MS) were performed. The calibration curves showed good linearities (above $r^2$ = 0.998) in the range of 5 ~ 1,000 ng/L. The method detection limit and the limit of quantification were 1.1 ~ 10.0 ng/L and 3.4 ~ 31.7 ng/L, respectively. Recoveries of the target compounds were between 70.1% and 115.8% (except cefadroxil, cefradine, vancomycin, and iopromide (50.2 ~ 67.0%)). The optimized analytical method can be useful to determine the residual pharmaceuticals in raw water.

Online preconcentration and preelutioin for the ion chromatographic determination of trace anions in high-sulfate wastewater

  • Song, Kyung-Sun;Kim, Sang-Yeon;Cheong, Young-Wook
    • 한국환경과학회:학술대회논문집
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    • 한국환경과학회 2005년도 봄 학술발표회지 제14권(제1호)
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    • pp.327-328
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    • 2005
  • Trace anions in high-sulfate wastewater from mainly derelict mines were determined by ion chromatography with on-line preconcentration and preelution technique. As the sample was preconcentrated and more strongly held ions were preeluted to the principal separation system, this approach was highly effective in removing large concentration of sulfate in high-sulfate wastewater. With this practical on-line preelution treatment, the peaks of fluoride and chloride showed good resolution even when the sulfate concentration was as high as 2000 mg/L and the analyzed total metal concentration was above 500 mg/L.

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