高效液相色谱-串联质谱法测定动物组织中的16种喹诺酮类药物残留

建立了动物组织样品中萘啶酸、恶喹酸、氟甲喹、诺氟沙星、依诺沙星、环丙沙星、洛美沙星、丹诺沙星、恩诺沙星、氧氟沙星、沙拉沙星、二氟沙星、麻保沙星、培氟沙星、司帕沙星、奥比沙星等16种喹诺酮类兽药多残留量的高效液相色谱-串联质谱测定方法。用酸性乙腈萃取样品中的16种喹诺酮类药物残留,然后用正己烷脱脂,旋转蒸发浓缩,以Inertsil C8-3色谱柱分离,在正离子模式下以电喷雾电离串联质谱进行测定。在10，50，100 μg/kg 3个加标水平下进行了验证试验,方法的线性范围为10~100 μg/kg,平均回收率为62.4%~102%,相对标准偏差为1.4%~11.9%。该方法简便、快速、准确,各项技术指标满足国内外法规的要求,可用于鸡肉、鸡肝和鱼肉等动物组织样品中喹诺酮类药物多残留的确证检测。

Determination of 16 Quinolone Residues in Animal Tissues Using High Performance Liquid Chromatography Coupled with Electrospray Ionization Tandem Mass Spectrometry

A confirmative method was developed with high performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry (HPLC-MS/MS) to simultaneously detect 16 quinolone residues in animal tissues, which included nalidixinic acid, oxolinic acid, flumequine, norfloxacin, enoxacin, ciprofloxacin, lomefloxacin, danofloxacin, enrofloxacin, ofloxacin, sarafloxacin, difloxacin, marbofloxacin, pefloxacin, sparfloxacin and orbifloxacin. In the method, the 16 residues were extracted with acidified acetonitrile, cleaned-up with hexane, and concentrated with a rotary evaporator. Then the reconstituted sample solution was analyzed using HPLC-MS/MS in positive mode, with a Inertsil C8-3 column as the analytical column. The method was validated at 10, 50 and 100 microg/kg. The validation results were as follows: the linear ranges were from 10 to 100 microg/kg; the overall recoveries were from 62.4% to 102% with the relative standard deviations of 1.4%-11.9%. The method is simple, rapid, and accurate, and its performance could meet the requirements of the domestic and international legislation. The method is applicable to simultaneously confirm multi-residues of quinolones in animal tissues such as chicken muscle, chicken liver and fish muscle.