Determination of Five Halogenated Methyl Sulfonic Acids in Sludge from Municipal Sewage Treatment Plant by HPLC-MS/MS

KeyWord:halogenated methyl sulfonic acids  sewage sludge  high performance liquid chromatography-tandem mass spectrometry£¨HPLC-MS/MS£©

Abstract:

      A method of high performance liquid chromatography-tandem mass spectrometry£¨HPLC-MS/MS£©was presented for the determination of five halogenated methyl sulfonic acids£¨HMSAs£©in sludge from municipal sewage treatment plant.Through investigation on extract solvent£¬extraction method and times£¬the optimum conditions were obtained as follows:the mixture of methanol and water£¨1¡Ã1£¬by volume£©was selected as extraction solvent£¬samples were continually oscillated at 350 r/min for 1 hour£¬and extracted once.Under the optimized conditions£¬the extraction efficiencies were£¨48ª±4¡À2ª±8£©%£¬£¨68ª±3¡À0ª±9£©%£¬£¨81ª±0¡À4ª±8£©%£¬£¨38ª±0¡À1ª±1£©% and£¨99ª±1¡À1ª±2£©% for chloromethanesulfonic acid£¬dichloromethanesulfonic acid£¬trichloromethanesulfonic acid£¬bromomethanesulfonic acid and trifluoromethanesulfonic acid£¬respectively.The calibration curves for the analytes were linear in the range of 0ª±05-50 ¦Ìg¡¤kg-1 with their correlation coefficients£¨r£©larger than 0ª±991.The limits of detection£¨LOD£©of the method ranged from 0ª±003 to 0ª±018 ¦Ìg¡¤kg-1 for HMSAs£¬and the limits of quantitation£¨LOQ£©were in the range of 0ª±010-0ª±059 ¦Ìg¡¤kg-1.The spiked recoveries for HMSAs in sewage sludge were in the range of 73ª±8%-101% with relative standard deviations of 2ª±3%-12ª±5%.