Determination of Niclosamide and Its Degradation Products in Sediments with Accelerated Solvent Extraction/Liquid Chromatography-Tandem Mass Spectrometry

KeyWord:liquid chromatography tandem mass spectrometry£¨LC-MS/MS£©  niclosamide  degradation products  accelerated solvent extraction  sediment

Abstract:

      A method based on liquid chromatography-tandem mass spectrometry with accelerated solvent extraction£¨ASE/LC-MS/MS£© was developed for the analysis of niclosamide and its degradation products£¨5 chlorosalicylic acid and 2 chloro 4 nitroaniline£© in sediments.Extraction and cleanup were integrated into one step by accelerated solvent extraction£¨ASE£© with 5ª±0 g neutral alumina as within cell adsorbing material,and different temperatures and static times were optimized with acetonitrile-water£¨3¡Ã1,by volume£© as extraction solvents.Under the optimized conditions,the calibration curves for niclosamide and its degradation products were linear in the range of 0ª±1-20ª±0 ¦Ìg/L with their correlation coefficients£¨r£© more than 0ª±999.The limits of detection and quantitation of the method were in the ranges of 0ª±04-0ª±1 ¦Ìg/kg and 0ª±2-0ª±5 ¦Ìg/kg,respectively.The proposed method was applied in the trace analysis of niclosamide and its degradation products in sediments with average recoveries in the range of 93ª±5%-101ª±9% at 3 spiked levels of 0ª±5,1ª±0 and 2ª±0 ¦Ìg/kg,and relative standard deviations of 3ª±7%-6ª±7%.The method was simple,sensitive and reproducible,and was suitable for the analysis of real sample.