액-액 추출과 아세틸화 후 GC-MS를 이용한 물 중 phenol의 분석
Quantitative Determination of Phenol in Water Using GC-MS after Liquid-Liquid Extraction and Acetylation
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초록
이 연구에서 개발한 방법은 phenyl acetate 유도체를 만든 후 추출-정제-농축 단계로 분석하는 기존 phenol 분석 방법의 ‘추가적인 정제 과정 필요’ 및 ‘많은 양의 유해 용매 사용’이라는 단점을 보완할 수 있는 분석 방법이다. 이 방법은 phenol을 물로부터 액-액 추출한 후 생성한phenyl acetate 유도체를 소량의 용매로 추출한 후 바로GC-MS에 주입하여 분석할 수 있는 장점을 갖고 있다. 이 방법은 기존 방법과 유사한 수준의 반복성, 회수율, 직선성 및방법검출한계를 나타내었고, 분석 과정이 기존에 비해 더 간단하여 물 중의 phenol 및 페놀류 화합물를 분석하는 데에적합할 것으로 생각한다.
Abstract
BACKGROUND: The phenol concentrations in water samples were determined using gas chromatography after derivatization of the analyte to phenyl acetate followed by extraction using a large volume of solvent. However, this procedure requires an additional purification step and is not analytically efficient. METHODS AND RESULTS: In this study, phenol was first extracted from an acidified water sample using ethyl acetate and then acetylated using acetic anhydride in the presence of a small amount of water and K2CO3. The derivativewas extracted using 1mLof n-butyl acetate.One microliter of the extract was analyzed by GC-MS without further purification. The calibration curve showed good linearity with the r2 value of 0.9968. Themethod detection limit and the limit of quantitationwere estimated to be 0.18 μg/L and 0.56 μg/L, respectively. Repeatability (RSD, n=3) and recovery (n=3) were 9.1%-4.3% and 90.6%-110.5%, respectively. The concentrations of phenol in a fewsamples of streamwaterwere distributed in the range of 2.51-7.51 μg/L. CONCLUSION: This method is simpler and faster to implement than those currently utilized and shows high analytical reliability. It can be applied to the quantitative determination of phenol concentrations in surface water and groundwater samples.
참고문헌 (7)
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