HPLC-ESI-MS/MS检测河豚鱼中5种抗生素残留的方法

Determination of 5 Macrolide Antibiotics in Pufferfish Meat by HPLC-ESI-MS/MS

建立一种同时测定河豚鱼中林可霉素、竹桃霉素、红霉素、替米考星和泰乐菌素5种大环内酯类抗生素残留的方法。试样中残留的抗生素用Tris缓冲溶液提取,经Oasis HLB固相萃取柱净化后,用液相色谱-质谱/质谱仪检测和确证,内标法定量。结果表明:5种大环内酯类抗生素在0.002～0.050μg/mL范围内均呈线性关系,相关系数r为0.9977～1.0000;在0.002～0.010mg/kg范围内,样品平均加标回收率在78.9%～109.0%之间,重复性相对标准偏差在1.3%～5.3%之间,再现性相对标准偏差在5.2%～14.5%之间,5种大环内酯类抗生素定量限均为2.0μg/kg。

A method has been developed for the simultaneous determination of five marcolide antibiotic residues including lincomycin, oleandomycin, erythromycin, tilmicosin and tylosin in pufferfish meat. Five antibiotic residues in samples were extracted into Tris buffer. The extract was cleaned up on an Oasis HLB column. The antibiotic residues were determined and confirmed by LC-MS/MS and quantified by an internal standard method. The calibration curves of 5 antibiotics exhibited good linearity in the concentration range of 0.002- 0.0501ag/mL with a correlation coefficient range of 0.9977- 1.0000. The average recovery rates of the marcolide antibiotics from pufferfish samples at spike levels of 0.002-0.010 mg/kg was 78.9%- 109.0% with a relative standard deviation of 1.3% - 5.3% for repeatability and with a relative standard deviation of 5.2% - 14.5% for reproducibility. The detection limit was 2.0 μt g/kg for these 5 antibiotics.