反相高效液相色谱/质谱法同时测定鸡肉中5种喹诺酮药物残留

Simultaneous Determination of Residues of Five Quinolones in Chicken Muscle by Reversed Phase High Performance Liquid Chromatography with Quadrupole Rods Tandem Mass Spectrometric Detection

采用反相高效液相色谱／四级杆串联质谱（RP-HPLC／MS／MS）同时测定鸡肉中的5种喹诺酮药物（quinolones，QNs）。均质后的鸡肉样品采用磷酸盐缓冲溶液和乙腈的混和溶液提取。提取液经正己烷液-液分配（LLP）去除脂肪后，用C18固相萃取（SPE）柱净化，氨化甲醇洗脱，洗脱液用氮气吹干，流动相定容后，分析物采用LC／MS／MS电喷雾电离（ESI），正离子，多反应监测（MRM）模式检测，外标法定量。在添加浓度2．5～10μg/kg范围内，5种QNs的回收率在79．8％～95．1％之间；相对标准偏差（RSD）均小于11．7％。环丙沙星、丹诺沙星、恩诺沙星检出限（LOD）为0．5μg／kg，沙托沙星为1．0μg／kg，氟甲喹为0．1μg／kg。

A reversed phase high-performance liquid chromatography-quadrupole rods tandem mass spectrometric （RP-HPLC/MS/MS） method was established for simultaneous determination of residues of five quinolones in chicken muscle. Homogenized samples were extracted with phosphate buffer and acetonitrile. Extracts were first defatted by liquid-liquid partition （LLP） with n-hexane, and then cleaned by C18 solid phase extraction （SPE） cartridge. Analytes were eluted by ammonia methanol, reconstituted by mobile phase after dried under nitrogen. Identification and quantification were achieved by electro-spray ionization （ESI） in positive mode using multiple reaction monitoring （MRM）. The recoveries of five QNs were between 79.8% and 95.1% at spiked levels of 2.5 - 10 μg/kg. The RSDs of the method were less than 11.7%. Limits of detection for ciprofloxacin, danofloxacin and enrofloxacin were 0.5 μg/kg, and for sarafloxacin and flume-quine were 1.0 μg/kg and 0.1 μg/kg, respectively