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[目的]本试验研究建立常见17种磺胺和15种喹诺酮类药物残留量的液相色谱-电喷雾串联离子阱质谱测定方法。[方法]以稳定同位素氘代磺胺邻二甲氧嘧啶、氘代磺胺间二甲氧嘧啶作为内标,采用多反应监测定量。样品经过匀浆、超声波提取、甲醇溶液涡旋溶解残留物、正己烷涡旋混合离心后进行液相色谱-质谱分析。采用C18柱,MGⅡ色谱柱,以均含0.1%甲酸的水和甲醇、乙腈为流动相进行梯度洗脱。[结果]17种磺胺和15种喹诺酮类药物的线性范围为2.0~50μg/kg,相关系数r>0.995,平均回收率为83.3%~109.9%(添加水平为2.5~10μg/kg),相对标准偏差为2.1%~8.1%。本方法最低检出限均为2.0μg/kg,最低定量限均为4.0μg/kg。[结论]所建方法简便、快速、干扰少、特异性强,是磺胺和喹喏酮残留检测的理想方法。
[Objective] The research aimed to establish a liquid chromatography-electrospray ionization tandem mass spectrometry method for the determination of 17 common sulfonamides and 15 quinolones residues. [Method] With stable isotope deuterosulfamethoxine and deuterosulfamidomethoxine as internal standard, the multi-reaction monitoring and quantification was used. Samples were homogenized, sonicated, and vortexed in methanol to dissolve the residue. Hexane was vortexed and centrifuged for liquid chromatography-mass spectrometry analysis. A C18 column and MG Ⅱ column were used. The mobile phase consisted of 0.1% formic acid in water and methanol and acetonitrile as eluent. [Results] The linear range of 17 sulfonamides and 15 quinolones was 2.0 ~ 50μg / kg with the correlation coefficient r> 0.995. The average recoveries ranged from 83.3% to 109.9% (2.5 ~ 10μg / kg) Deviations of 2.1% ~ 8.1%. The minimum detection limit of this method are 2.0μg / kg, the minimum limit of quantification were 4.0μg / kg. [Conclusion] The established method is simple, rapid, less interference and strong specificity, which is an ideal method for the determination of sulfonamides and quinuclidine residues.