토양 중 음이온 바이오사이드의 HPLC-MS/MS 동시 정량분석법
Simultaneous and quantitative determination of anion biocides in soil by liquid chromatography-tandem mass spectrometry
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초록
토양 중 음이온 바이오사이드인 chlorite, chlorate, cyanuric acid와 sodium dodecylbenzenesulfonate (Na-DBS)의 liquid chromatography-tandem mass spectrometry (LC-MS/MS) 동시 분석방법을 개발하였다. Chlorite와 chlorate는 물로 추출하였으며, cyanuric acid와 Na-DBS는 0.25 mM ammonium formate를 함유한 20 mM formic acid와 acetonitrile (1:1) 이동상을 이용하여 추출하였다. 추출물은 필터 후 직접 LCMS/ MS로 주입하였다. 분석물질이 검출되지 않는 토양에 각 성분들을 첨가한 후 정도관리를 실시한 결과 검출한계는 chlorite 0.04 mg/kg, chlorate 0.04 mg/kg, cyanuric acid 0.27 mg/kg 그리고 Na-DBS의 경우는 0.05 mg/kg 이었다. 이 방법을 사용하여 우리나라 AI로 소독제를 많이 사용한 장소 40개 지역과 사용하지 않은 지역 10개 대조 지역의 토양을 분석한 결과 대조지역을 포함한 모든 조사지역에서 네 가지음이온 모두 검출되지 않았다.
Abstract
Simultaneous analytical method has developed for the determination of anion biocides in soil by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Chlorite and chlorate in soil were extracted with pure water, and cyanuric acid and sodium dodecylbenzenesulfonate (Na-DBS) were extracted with mobile phase (0.25 mM ammonium formate in 20 mM formic acid : acetonitrile (1:1)). The extract was injected into the LC-MS/MS system after filtration. The method detection limits in this study were 0.04 mg/kg for chlorite, 0.04 mg/kg for chlorate, 0.27 mg/kg for cyanuric acid, and 0.05 mg/kg for Na-DBS, respectively. The method was applied to the analysis of 50 soil samples collected from 40 sites sprayed with biocides and 10 background sites. As a result, anion biocides were not detected in all sites.
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