나뭇잎에 침착된 PAHs 분석법 개발
Development of Analytical Method of PAHs Deposited on Tree Leaves
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A simple, effective and economic method for clean-up samples to analyse PAHs deposited on pine needles was developed as follows. The juice was extracted from 4~5 g of pine needles cut into about 2 cm, twice with 50 mL of dichloromethane (DCM) in ultrasonicator for 1 hr, followed by collection and concentration using a rotary vacuum evaporator into 2~3 mL. The extract was passed through an 11 mm wide and 230 mm long glass column (packed from the bottom with 2.5 g of alumina, 1.5 g of silica and 2 g of sodium sulfate, and baked at 250 for 12 h) with a 70 mL of mixture of hexane: DCM (1:1). The eluate was concentrated into 1 mL by a rotary vacuum evaporator, and performed clean-up with an 80 mL of mixture hexane:DCM (1:1) using a 20 mm wide and 220 mm long GPC column packed with 12 g of Bio-beads. The first 37 mL of the eluate containing interferences was removed, and the latter 43 mL containing PAHs was collected and concentrated into 1~2 mL using a rotary vacuum evaporator, and transferred volumetric to a vial. Nonane was added as a keeper, followed by enrichment by nitrogen into 50 μL on a hot plate for the GC-MS analysis. The estimation using the deuterated PAHs found the recoveries of the whole procedure as 42~105.1% (the coefficients of variation 5.3~14.8%). As decreasing the molecular weight, the recoveries decreased and the coefficients of variation increased.
Abstract
A simple, effective and economic method for clean-up samples to analyse PAHs deposited on pine needles was developed as follows. The juice was extracted from 4~5 g of pine needles cut into about 2 cm, twice with 50 mL of dichloromethane (DCM) in ultrasonicator for 1 hr, followed by collection and concentration using a rotary vacuum evaporator into 2~3 mL. The extract was passed through an 11 mm wide and 230 mm long glass column (packed from the bottom with 2.5 g of alumina, 1.5 g of silica and 2 g of sodium sulfate, and baked at 250 for 12 h) with a 70 mL of mixture of hexane: DCM (1:1). The eluate was concentrated into 1 mL by a rotary vacuum evaporator, and performed clean-up with an 80 mL of mixture hexane:DCM (1:1) using a 20 mm wide and 220 mm long GPC column packed with 12 g of Bio-beads. The first 37 mL of the eluate containing interferences was removed, and the latter 43 mL containing PAHs was collected and concentrated into 1~2 mL using a rotary vacuum evaporator, and transferred volumetric to a vial. Nonane was added as a keeper, followed by enrichment by nitrogen into 50 μL on a hot plate for the GC-MS analysis. The estimation using the deuterated PAHs found the recoveries of the whole procedure as 42~105.1% (the coefficients of variation 5.3~14.8%). As decreasing the molecular weight, the recoveries decreased and the coefficients of variation increased.
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