고분해능 질량분석장치를 이용한 수중 피레스로이드계 농약성분 동시분석
Applications of High Resolution Mass Spectrometer for Simultaneous Quantitation of Pyrethroid Pesticides in Water
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초록
A gas chromatography-high resolution mass spectrometry (GC-HRMS) method with solid-phase extraction has been developed to simultaneously quantitate pyrethroid pesticides in water samples. Target compounds in this study were permethrin, cypermethrin, fenpropathrin, cyhalothrin(-l, -g), cyfluthrin, tefluthrin, flucythrinate and bifenthrin. To improve sensitivities of the method for pyrethroid pesticides, framgment ions were surveyed to select a quantification mass with the second prior mass or molecular mass as a qualificator. Deuterium poly aromatic hydrocarbons like phenanthrene-d10 and perylene-d12 were added as a internal standards. Prior to sample analysis, disk type solid-phase extraction was validated using RPS and C18 for raw and treated water. Higher average recoveries ranged from 80% to 87% were observed in C18 disk for raw and treated water. Performance test of SPE-GC-HRMS method for pyrethroid pesticides were carried out with samples spiked with target compounds at 5 ng/L each. Method detection limits (MDLs) were 0.90~7.45 ng/L with the accuracy of 71~98% and the precision of 7.2~10.4% exept for cypermethrin(21.8%). The developed method was applied to quantitate the residual pesticides in river water (n=3), surface water from apple farm (n=2) and tap water (n=5). Target compounds were not detected from all samples, but interfering peaks caused by similar fragments with different retention times were observed.
Abstract
A gas chromatography-high resolution mass spectrometry (GC-HRMS) method with solid-phase extraction has been developed to simultaneously quantitate pyrethroid pesticides in water samples. Target compounds in this study were permethrin, cypermethrin, fenpropathrin, cyhalothrin(-l, -g), cyfluthrin, tefluthrin, flucythrinate and bifenthrin. To improve sensitivities of the method for pyrethroid pesticides, framgment ions were surveyed to select a quantification mass with the second prior mass or molecular mass as a qualificator. Deuterium poly aromatic hydrocarbons like phenanthrene-d10 and perylene-d12 were added as a internal standards. Prior to sample analysis, disk type solid-phase extraction was validated using RPS and C18 for raw and treated water. Higher average recoveries ranged from 80% to 87% were observed in C18 disk for raw and treated water. Performance test of SPE-GC-HRMS method for pyrethroid pesticides were carried out with samples spiked with target compounds at 5 ng/L each. Method detection limits (MDLs) were 0.90~7.45 ng/L with the accuracy of 71~98% and the precision of 7.2~10.4% exept for cypermethrin(21.8%). The developed method was applied to quantitate the residual pesticides in river water (n=3), surface water from apple farm (n=2) and tap water (n=5). Target compounds were not detected from all samples, but interfering peaks caused by similar fragments with different retention times were observed.
참고문헌 (16)
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