超高效液相色谱-电喷雾串联四极杆质谱法检测牛奶中22种喹诺酮类抗菌素

应用液相色谱-电喷雾串联四极杆质谱仪,检测牛奶中的喹诺酮类(QNs)抗菌素.样品经柠檬酸磷酸盐缓冲液(Mcllvaine)超声提取,采用固相萃取(SPE)方法净化提取液并对目标物质进行富集,用UPLC-MS/MS检测.实验通过空白基质溶液稀释标准,建立校正的标准曲线,可以降低基质对离子化的干扰.结果表明:吡哌酸、依诺沙星、西诺沙星、奥索利酸在3～300 μg/kg,帕珠沙星在5～500 μg/kg,氧氟沙星、加替沙星、司帕沙星在0 5～50 μg/kg,其余14种喹诺酮类化合物在1～100 μg/kg的线性范围内均具有良好的线性关系,相关系数在0 9851～0 9997之间,定量限(LOQ)为0 008～0 339 μg/kg.除了氟甲喹、萘啶酸、那氟沙星的回收率小于60%外,其它喹诺酮的回收率均在63.1%～94.6%之间,相对标准偏差为0 86%～13.12%.

Determination of 22 Quinolones Antibiotics Residues in Milk by Ultra Performance Liquid Chromatography with Electrospray Ionization Tandem Mass Spectrometric Detection

The ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS) method has been developed for 22(fluoro)quinolone(QNs) antibiobtics in milk with multiple reaction monitoring(MRM).The analytes were extracted from the sample using Mcllvaine buffer by ultrasonic bath,and purified by solid-phase extraction(SPE) cartridge.The residue was dried under nitrogen and dissolved to UPLC-MS/MS.The interference of matrix was reduced by the matrix-matched calibration standards curve.The linear range was f...