UPLC-MS/MS法同时检测水产品中喹诺酮类药物残留

Simultaneous Determination of Quinolones in Aquatic Products by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

利用UPLC-MS/MS技术建立一种同时检测水产品中喹诺酮类药物残留的分析方法。对样品进行前处理及分离条件的优化,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法检测。结果表明:依诺沙星、奥索利酸、培氟沙星、帕珠沙星、氟罗沙星含量在3～300μg/kg范围,萘啶酸、氟甲喹含量在0.5～50μg/kg范围,其余13种喹诺酮类化合物含量在l～100μg/kg范围均具有良好的线性关系,相关系数0.9981～0.9999,定量限(LOQ)0.34～8.13μg/kg。药物含量在5～150μg/kg范围,除氟甲喹、萘啶酸外,其它喹诺酮的回收率均在63.6%～92.8%之间,相对标准偏差1.51%～11.32%。该方法可满足水产品中喹诺酮类药物多残留检测的要求。

An ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）method was developed for the trace analysis and validation of 20 quinolones in aquatic products.Pretreatment and isolation conditions of sample were optimized.The analytes were extracted from the samples using Mcllvaine buffer by ultrasonic bath,and purified and enriched by solid-phase extraction（SPE）cartridge,and detected by UPLC-MS/MS.The results showed that the linear range was from 3 μg/kg to 300 μg/kg for enrofloxacin,oxolinic acid,Pefloxacin,Pazufloxacin,Fleroxacin,from0.5 μg/kg to 50 μg/kg for Nalidixic acid,Flimequine,from 1 μg/kg to 100 μg/kg for other 14 QNs with the good correlation coefficients（r≥0.9981）.The lower limit of quantification was 0.34 μg/kg to 8.13 μg/kg.The recoveries were 63.6%～92.8%,except for FLU and NAL with relative standard deviations of 1.51%～11.32%,respectively,in spiked tissue samples at concentration levels ranging from 2.5 μg/kg to 150 μg/kg of each quinolone.The method is simple,accurate and sensitive for the simultaneous determination of various QNs in aquatic products.