超高效液相色谱串联三重四极杆质谱测定蜂蜜中氯霉素残留

摘要

Objective To establish a method for the determination of chloramphenicol residue in honey by ultra performance liquid chromatography/triple quadruple tandem mass spectrometry.Methods Samples were extracted using ethyl acetate,purified by solid phase extraction column and separated on a Waters BEH C18 column(2.1 mm× 100 mm,1.7 μm)with a mobile phase composed of 0.05％ ammonia and acetonitrile.The analysis was carried out with internal standard quantitative method by MS/MS in an electrospray positive ion multiple reaction monitoring (MRM) mode.Results The limits of detection and limit of quantitation were 0.01 ng/mL and 0.1 μg/kg,respectively.The recovery was 92％～105％ at 0.01～5.0 ng/mL,and the relative standard deviation was less than 4％.Conclusion The method is rapid,sensitive and specific,which is suitable for determination of supervision in honey.%目的 建立超高效液相色谱串联三重四极杆质谱法测定蜂蜜中氯霉素残留的分析方法.方法 样品经乙酸乙酯提取,过固相萃取小柱净化,用Waters BEH C18柱(2.1 mm×100 mm,1.7 μm)分离,流动相为0.05％氨水/乙腈梯度洗脱,内标法定量,电喷雾离子MRM(multiple reaction monitoring)模式检测.结果 该方法的检出限为0.01 ng/mL,样品的定量限为0.1 μg/kg,线性范围为0.01～5.0 ng/mL,平均回收率为92％～105％,相对标准偏差小于4％.结论 该方法灵敏、准确、快速,能满足蜂蜜中氯霉素的监督检测.