시료 농축 후 액-액-추출과 GC-MS를 이용한 염소 소독 음용수중 3-chloro-4-(dichloromethyl)-5-hydroxy-2(5H)-furanone(MX)의 정량 분석
Quantitative determination of 3-chloro-4-(dichloromethyl)-5-hydroxy-2(5H)- furanone (MX) in chlorinated drinking water using sample enrichment followed by liquid-liquid extraction and GC-MS
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초록
염소로 소독된 음용수에서 수백 ng/L의 농도까지 검출되는 3-chloro-4-(dichloromethyl)-5-hydroxy- 2(5H)-furanone(MX)를 시료 농축 후 액-액 추출(LLE), 메틸 유도체화 및 GC-MS로 정량 분석하였다. 4 L의 물 시료를 감압회전증발기를 사용해 30 oC에서 0.4 L로 농축하였다. 물 중의 MX는 ethyl acetate (100 mL × 2)를 용매로 사용하여 추출하였으며, 추출액 중 MX는 10 % H2SO4 in methanol로 methyl 유도체를 만들었다. MX의 회수율은 73.8%이었으며, 이는 수지 흡착법의 38.1%보다 높았다. 정량한계와반복성(RSD)은 각각 10 ng/L와 2.2%로 추정되었다. 이 결과는 시간이 더 많이 소요되는 수지 흡착법의대체 방법으로 LLE가 사용될 수 있다는 것을 보여 주었다.
Abstract
This study explores the means by which MX can be effectively extracted from chlorinated water 3-Chloro-4-(dichloromethyl)-5-hydroxy-2(5H)-furanone (MX), a potent mutagen commonly found in chlorinated drinking water at concentrations of up to a few hundred ng/L, was quantitatively determined using sample enrichment followed by liquid-liquid extraction (LLE), derivatization to methylated form, and analysis with GC-MS. A 4-L water sample was enriched to a concentration of 0.4 L using a vacuum rotary evaporator at 30 oC. MX in the water was extracted using ethyl acetate (100 mL × 2) as a solvent and MX in the extract was methylated with 10% H2SO4 in methanol. MX was recovered at a rate of 73.8 %, which was higher than that (38.1 %) for the resin adsorption method. The limit of quantification and repeatability (as relative standard deviation) were estimated to be 10 ng/L and 2.2%, respectively. This result suggested that LLE can be used for the determination of MX in chlorinated water as an alternative to more time-consuming resin adsorption method.
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