Simultaneous Determination of Tetracycline, Macrolide and Sulfonamide Antibiotics in Soils Using Accelerated Solvent Extraction Followed by Solid-Phase Extraction and High Performance Liquid Chromatography Tandem Mass Spectrometry

摘要

This research developed and optimized the methods for simultaneous determination of tetracycline (TCs), macrolide (MLs) and sulfonamide (SAs) antibiotics in soils using accelerated solvent extraction(ASE)- solid- phase extraction (SPE)-high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS). Methanol-citric acid (pH=4.7) was used as extraction solvent, diatomite (washed by EDTA) was used as dispersing agent. Firstly, soil was extracted by ASE with the parameter conditions: pressure 1500 psi, temperature 70°C, static 10 min, 1 circle, then pre-concentration by SPE and followed by HPLC-MS/MS analysis. Recovery was 86.3%～97.4% for SAs, 67.3%～87.4% for TCs and 68.4%～78.3% for MLs. RSD < 9 % and r > 0.99. Limits of detection (LOD) was 0.5～0.9 ug/kg for SAs, 0.2～1.1 ug/kg for TCs and 0.2～0.3 ug/kg for MLs. This method determined 9 kinds of antibiotics within 15 min, the determination accuracy can meet the requirements of actual analysis.