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

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Research article

Journal of the Korean Society for Environmental Analysis 2008;11(3):222-231.

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

최재원¹, 김정희², 김용연², 정팔진³

¹한국수자원공사 수자원연구원
²한국수자원공사
³전북대학교

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.

Key Words: Perfluorinated compounds (PFCs), PFOS, PFOA, Solid-phase extraction (SPE), Liquid chromatograph- triple quadrupole mass spectrometer (LC-MS/MS), Water