Determination of Niclosamide and Its Degradation Products in Sediments with Accelerated Solvent Extraction/Liquid Chromatography-Tandem Mass Spectrometry
Determination of Niclosamide and Its Degradation Products in Sediments with Accelerated Solvent Extraction/Liquid Chromatography-Tandem Mass Spectrometry[J]. 2018,37(7):825-829.
Determination of Niclosamide and Its Degradation Products in Sediments with Accelerated Solvent Extraction/Liquid Chromatography-Tandem Mass Spectrometry[J]. 2018,37(7):825-829.DOI:
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 50 g neutral alumina as within cell adsorbing material,and different temperatures and static times were optimized with acetonitrile-water(3∶1,by volume) as extraction solvents.Under the optimized conditions,the calibration curves for niclosamide and its degradation products were linear in the range of 01-200 μg/L with their correlation coefficients(r) more than 0999.The limits of detection and quantitation of the method were in the ranges of 004-01 μg/kg and 02-05 μg/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 935%-1019% at 3 spiked levels of 05,10 and 20 μg/kg,and relative standard deviations of 37%-67%.The method was simple,sensitive and reproducible,and was suitable for the analysis of real sample.
关键词
液相色谱-串联质谱法(LC-MS/MS)氯硝柳胺降解产物加速溶剂萃取底泥
Keywords
liquid chromatography tandem mass spectrometry(LC-MS/MS)niclosamidedegradation productsaccelerated solvent extractionsediment