超高效液相色谱-串联质谱法同时测定鳗鱼中32种兽药残留

Simultaneous determination of 32 kinds of veterinary drug residues in eels by ultra performance liquid chromatography-tanderm mass spectrometry

中文关键词:  鳗鱼  超高效液相色谱-串联质谱法  磺胺类  喹诺酮类  四环素类

英文关键词:eels  ultra performance liquid chromatography-tandem mass spectrometry  sulfonamides  quinolones  tetracyclines

中文摘要:

      目的 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)同时测定鳗鱼中13种磺胺类、15种喹诺酮类和4种四环素类兽药残留的分析方法。方法 鳗鱼试样采用乙二胺四乙酸二钠(ethylenediaminetetraacetic acid disodium salt, Na2EDTA)-Mcllvaine提取液进行提取, HLB固相萃取柱净化, Waters ACQUITY UPLC BEH C18色谱柱分离, 以0.1%甲酸乙腈和0.1%甲酸水溶液作为流动相进行梯度洗脱; 电喷雾正离子模式下, 以多反应监测(multiple reaction monitoring, MRM)方式采集数据进行定性与定量分析, 外标法定量。结果 磺胺类、喹诺酮类及四环素类药物分别在2~50、2~50、5~100 μg/kg浓度范围内线性相关性良好, 相关系数均大于0.99; 不同加标水平的平均回收率为82.6%~110.2%, 相对标准偏差(relative standard deviations, RSDs)为3.2%~13.9%, 检出限(limits of detection, LODs)和定量限(limits of quantification, LOQs)分别为0.3~2.0 μg/kg和1.0~5.0 μg/kg。结论 本方法快速简便、灵敏可靠, 适合大批量鳗鱼中同时快速对磺胺类、喹诺酮类及四环素类兽药残留进行定性和定量检测。

英文摘要:

      Objective To establish a method for the simultaneous determination of 13 kinds of sulfonamides, 15 kinds of quinolones and 4 kinds of tetracyclines residues in eels by ultra performance liquid chromatography-tanderm mass spectrometry (UPLC-MS/MS). Methods The analytes were extracted with ethylenediamine tetraacetic acid disodium salt (Na2EDTA)-Mcllvaine buffer, then purified with HLB solid phase extraction columns, and analyzed by Waters ACQUITY UPLC BEH C18 column with gradient elution using acetonitrile (containing 0.1% formic acid) and 0.1% formic acid solution as the mobile phase. The analytes were detected with electrospray ionization in the positive mode using multiple reaction monitoring (MRM) for the qualitative and quantitative analysis. The compounds were quantitatively analyzed by external standard method. Results The linear relationships of the sulfonamides, quinolones and tetracyclines were good within the concentration range of 2?50, 2?50, 5?100 μg/kg respectively, and the correlation coefficients were larger than 0.99. The average recoveries were 82.6%?110.2%, the relative standard deviations (RSDs) were 3.2%?13.9%, the limits of detection (LODs) were 0.3?2.0 μg/kg, and the limits of quantification (LOQs) were 1.0?5.0 μg/kg. Conclusion This method is fast, simple, sensitive and reliable. It is a qualitative and quantitative method suitable for the quick and simultaneous determination of sulfonamides, quinolones and tetracyclines veterinary drug residues in large quantities of eels.