QuEChERS-高效液相色谱-质谱联用法同时检测鸡胗和鸡肝中15种喹诺酮类和四环素类抗生素

Simultaneous Determination of 15 Quinolones and Tetracyclines Antibiotics in Chicken Gizzard and Liver by QuEChERS-High Performance Liquid Chromatography-Mass Spectrometry

为建立可以同时准确检测鸡胗和鸡肝中11种喹诺酮类和4种四环素类抗生素的分析方法,采用QuEChERS(quick,easy,cheap,effective,rugged,safe)法进行样品前处理,经过冰乙酸-乙腈-水溶液(1∶84∶15,V/V)提取,Discovery^?DSC-18吸附剂净化,使用高效液相色谱-质谱联用仪进行检测,选用甲醇-0.1%甲酸体系作为流动相对目标物进行梯度洗脱,采用多反应监测模式进行检测。结果表明:15种抗生素在质量浓度2~80 ng/mL范围内与其响应值存在良好的线性关系(R^2≥0.9933),方法检出限为0.5~3.0μg/kg,定量限为1.7~10.0μg/kg,平均加标回收率为75.2%~104.4%,相对标准偏差为2.7%~8.7%;随机抽取100份样品(其中鸡胗样品51份,鸡肝样品49份)用上述方法进行检测,15种抗生素的总体检出率为21.38%,残留量为3.48~154.00μg/kg。

A method which can simultaneously determine the residues of 11 quinolones and 4 tetracyclines antibiotics in chicken gizzard and liver was established using high performance liquid chromatography-mass spectrometry(HPLC-MS).The samples were pretreated by the widely used QuEChERS(quick,easy,cheap,effective,rugged,safe)method and extracted with glacial acetic acid-acetonitrile-water(1:84:15,V/V),and then extract was cleaned up using Discovery^? DSC-18 sorbent,separated using methanol as mobile phase A and 0.1%formic acid in water as mobile phase B by gradient elution,and detected in the multiple reaction monitoring(MRM)mode.There were good linear relationships between the concentrations of the 15 antibiotics in the range of 2–80 ng/mL and their response values(R^2≥0.9933).The detection limits of this method were 0.5–3.0μg/kg and the quantitation limits were 1.7–10.0μg/kg.The average recovery of spiked samples was 75.2%–104.4%with relative standard deviation(RSD)of 2.7%to 8.7%.When 51 chicken gizzard samples and 49 chicken liver samples were randomly chosen and tested by this method,the total detection rate of the 15 antibiotics was 21.38%and their residual levels were 3.48–154.00μg/kg.