Yue Zhenfeng, Lin Xiuyun, Tang Shaobing, Chen Xiaoxia, Ji Caini, Hua Honghui, Liu Yu
Food Inspection and Quarantine Center, Shenzhen Entry-Exit Inspection & Quarantine Bureau, Shenzhen 518067, China.
Se Pu. 2007 Jul;25(4):491-5.
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.
建立了一种高效液相色谱-电喷雾电离串联质谱联用(HPLC-MS/MS)的确证方法,用于同时检测动物组织中的16种喹诺酮类药物残留,包括萘啶酸、恶喹酸、氟甲喹、诺氟沙星、依诺沙星、环丙沙星、洛美沙星、达氟沙星、恩诺沙星、氧氟沙星、沙拉沙星、二氟沙星、马波沙星、培氟沙星、司帕沙星和奥比沙星。该方法中,16种残留用酸化乙腈提取,用正己烷净化,并用旋转蒸发仪浓缩。然后将复溶后的样品溶液采用HPLC-MS/MS正离子模式进行分析,以Inertsil C8-3柱作为分析柱。该方法在10、50和100μg/kg三个添加水平进行了验证。验证结果如下:线性范围为10~100μg/kg;总回收率为62.4%~102%,相对标准偏差为1.4%~11.9%。该方法简便、快速、准确,其性能能够满足国内外法规的要求。该方法适用于同时确证鸡肌肉、鸡肝和鱼肌肉等动物组织中喹诺酮类药物的多残留。