title: High-performance liquid chromatography-fluorescence determination of dinitropyrenes in soil after column chromatographic clean-up and on-line reduction.
abstract: In order to quantify 1,3-dinitropyrene (DNP), 1,6-DNP and 1,8-DNP in soil, we developed an efficient clean-up procedure and a sensitive determination method using fluorescence detection. DNP isomers were efficiently cleaned by three stages of fractionation, i.e., a silica gel open column chromatography using stepwise elution and two further purification steps by high-performance liquid chromatography (PPLC) using a monomeric-type octadecylsilyl (ODS) column and a polymeric-type ODS column. The recoveries of DNPs during the whole clean-up process were 94% or more. The fraction corresponding to DNPs was injected into an analytical polymeric-type ODS column for HPLC to separate DNP isomers. The effluent from the analytical ODS column was directly introduced to a catalyst column, which was packed with 5 microns alumina coated with platinum and rhodium (Pt-Rh), in order to reduce DNPs to diamino compounds, and then the fluorescence of diaminopyrenes was detected. The immediate detection of diaminopyrene isomers after on-line reduction afforded a sensitive detection of DNP isomers. The detection limits for DNPs were in the range of 0.7 to 4 pg. These developed methods were applied to four soil samples collected at parks in residential areas.
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D009153:Mutagens / Q000032:analysis*; D011721:Pyrenes / Q000032:analysis*; D012680:Sensitivity and Specificity; D012987:Soil / Q000032:analysis*; D012989:Soil Pollutants / Q000032:analysis; D013050:Spectrometry, Fluorescence; D013056:Spectrophotometry, Ultraviolet