| Popis: |
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. |
