超高效液相色谱三重四极杆质谱法快速测定蜂蜜中12种大环内酯和林可酰胺类药物残留

Rapid multiresidue analysis of 12 macrolides and lincoamides in honey by ultra performance liquid chromatography coupled with triple quadrupole mass spectrometry

目的:应用超高效液相色谱串联质谱联用技术,建立了蜂蜜中12种大环内酯和林可酰胺类抗生素的多残留检测方法。方法:样品用2 mol/L乙酸铵水溶液调节pH值至中性,然后用20%甲醇水超声溶解、高速离心、ACQUITY UP-LC HSS T3色谱柱分离后串联质谱电喷雾正离子多反应监测模式检测,基质匹配标准内标法定量。结果:大环内酯和林可酰胺类抗生素残留的检测限为0.1μg/kg～1.0μg/kg(S/N=3),定量限为0.3μg/kg～3.0μg/kg。平均加标回收率在94%～115%之间,相对标准偏差1.3%～14.7%(n=6)。结论:本法简便、灵敏、准确,能够快速确证检测蜂蜜中12种大环内酯和林可酰胺类抗生素的残留。

Objective：To develop a simple and rapid method for the determination of 12 macrolides and lincoamides residues in honey by ultra-performance liquid chromatography-tandem mass spectrometry.Methods：Samples were first adjusted to neutral and then dissolved in 20% methanol solution.After being separated on an ACQUITY UPLC HSS T3 column,the analytes were detected by positive electrospray ionization-tandem mass spectrometry in the MRM mode and quantified by matrix-match internal standard method.Results：The limits of detection and limits of quantitaion for the 12 compounds were within 0.1 μg/kg～1.0 μg/kg and 0.3 μg/kg～3.0 μg/kg,respectively.The average recoveries for the macrolides and lincoamides ranged from 94% to 115% with the relative standard deviation（RSD） of 1.3%～14.7%（n=6）.Conclusion：This method is simple,sensitive and accurate to confirmatively detect the 12 macrolides and lincoamides residues in honey.