超高效液相色谱-串联质谱测定淤泥4种氟喹诺酮类药物残留An Analysis of 4 Kinds of Residual Fluoroquinolones in Silt by Using Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry
符靖雯;吴育彬;刘惠茹;杨钦沾;
摘要(Abstract):
应用超高效液相色谱-串联质谱(UPLC-MS/MS)同时检测淤泥中氧氟沙星、环丙沙星、恩诺沙星和达氟沙星4种氟喹诺酮类药物的残留量.针对所检测样品的化学性质,对色谱的条件、提取剂和稀释条件等参数进行了优化.最终以加入Na2EDTA的乙腈:磷酸盐缓冲液(1:1)(pH=3)作为提取剂,经超声处理、SAX-HLB串联固相萃取小柱富集净化,以Agilent C_(18)色谱柱进行分离,采用0.2%甲酸水溶液(5 mmoL/L乙酸铵)、0.2%甲酸甲醇作为流动相,在UPLC-MS/MS多反应监测模式(MRM)下检测,基质曲线外标法定量.结果表明,4种氟喹诺酮类药物在5 ng/mL100 ng/mL浓度范围内线性关系良好,相关系数均>0.998,方法检出限为0.015100 ng/mL浓度范围内线性关系良好,相关系数均>0.998,方法检出限为0.0150.060μg/kg.4种氟喹诺酮类药物在低、中、高3个加标水平中的平均回收率为70.4%0.060μg/kg.4种氟喹诺酮类药物在低、中、高3个加标水平中的平均回收率为70.4%89.4%,相对标准偏差(RSD)为7.4%89.4%,相对标准偏差(RSD)为7.4%9.4%.本方法简单、快速,灵敏度高,适用于养殖场淤泥中四种痕量抗生素残留检测.
关键词(KeyWords): 超高效液相色谱-串联质谱;测定;淤泥;氟喹诺酮类
基金项目(Foundation): 惠州市科技计划项目(2016X0419034)
作者(Authors): 符靖雯;吴育彬;刘惠茹;杨钦沾;
DOI: 10.16778/j.cnki.1671-5934.2018.03.005
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