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SPE-LC-MS/MS에 의한 과불화화합물의 수질분석 - 고상추출법 비교를 중심으로 -

Development of an Analytical Method for the Determination of Perfluorinated Compounds by the Assays of Solid-phase Extraction and LC-MS/MS

김정희|김용연|최재원|정팔진
한국환경분석학회 (The Korean Society For Environmental Analysis)|2008.09|환경분석과 독성보건 (JOURNAL OF ENVIRONMENTAL ANALYSIS, HEALTH AND TOXICOLOGY)|제11권 제3호|pp. 222-231

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참고문헌

키워드

WaterPFOSPFOAPerfluorinated compounds (PFCs)Solid-phase extraction (SPE)

초록

Solid-phase extraction (SPE) was assayed in combination with liquid chromatography - tandem mass spectrometry (LC-MS/MS) for analysing perfluorooctanoic acid (PFOA), perfluorononanoic acid (PFNA), perfluorodecanoic acid (PFDA), perfluoro-7-methyloctanoic acid (PFOA-7methyl), perfluoroctanesulfonate (PFOS), perfluorodecanesulfonate (PFDS) and perfluorodecanesulfinate (PFDSi) in raw water sample from drinking water treatment plants. Once, the optimization of MS/MS fragmentation analysis was carried out, sample extraction method was compared using the six SPE cartridges, and the determination of linearity, accuracy, precision and method detection limits (MDLs) were performed. SPE-LC-MS/MS method described enabled us to determine the target compounds at 0.2~2.4 ng/L levels. PFNA and PFOA-7methyl which have the same precursor and product ion mass showed chromatographic separation in the LC column. In sample extraction, adopting the washing fraction to remove interferences should be validated carefully. In SPE validation, HLB, 8B-S100-FCH and 8B-S100-FBJ is recommended, but some types of cartridge showed unreasonable high recoveries. Method blanks including field and reagent blank should be validated for real sample analysis to avoid the over-estimated values.

Abstract

Solid-phase extraction (SPE) was assayed in combination with liquid chromatography - tandem mass spectrometry (LC-MS/MS) for analysing perfluorooctanoic acid (PFOA), perfluorononanoic acid (PFNA), perfluorodecanoic acid (PFDA), perfluoro-7-methyloctanoic acid (PFOA-7methyl), perfluoroctanesulfonate (PFOS), perfluorodecanesulfonate (PFDS) and perfluorodecanesulfinate (PFDSi) in raw water sample from drinking water treatment plants. Once, the optimization of MS/MS fragmentation analysis was carried out, sample extraction method was compared using the six SPE cartridges, and the determination of linearity, accuracy, precision and method detection limits (MDLs) were performed. SPE-LC-MS/MS method described enabled us to determine the target compounds at 0.2~2.4 ng/L levels. PFNA and PFOA-7methyl which have the same precursor and product ion mass showed chromatographic separation in the LC column. In sample extraction, adopting the washing fraction to remove interferences should be validated carefully. In SPE validation, HLB, 8B-S100-FCH and 8B-S100-FBJ is recommended, but some types of cartridge showed unreasonable high recoveries. Method blanks including field and reagent blank should be validated for real sample analysis to avoid the over-estimated values.

참고문헌 (31)

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