[目的] 建立一种超高效液相色谱-串联质谱法（UPLC-MS/MS）快速检测牛奶中酰胺醇类抗生素残留的方法,要求可同时检测氯霉素、甲砜霉素、氟苯尼考及其主要代谢物氟苯尼考胺,且具有较低的检出限。[方法] 牛奶经三氯乙酸溶液沉淀蛋白,氨化乙酸乙酯提取,MCX固相萃取柱净化,甲醇-水溶液复溶,Waters ACQUITY UPLC HSS T3色谱柱（2.1 mm×100 mm,1.8 μm）分离,以25%甲醇（A流路）和75%水（在200 mL水中加入100 μL5%氨化甲醇溶液,B流路）作为流动相进行梯度洗脱。采用多反应监测（MRM）进行质谱分析,外标法定量。[结果] 该法可在5 min内完成4 种酰胺醇类化合物的检测。4 种酰胺醇类化合物在0.3、0.6、1.5 μg/kg的添加水平上回收率为77.3%~106.4%,相对标准偏差范围为1.6%~11.8%（n=6）,方法检出限为0.1 μg/kg,定量限为0.3 μg/kg。[结论] 该法全面、快速、准确度好、灵敏度高、稳定,适用于牛奶中4 种酰胺醇类抗生素残留的检测。

[Objective] To establish a rapid method for ultra-high performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS） detection of amphenicol antibiotic residues in milk. The method should be capable of simultaneously detecting chloramphenicol,thiamphenicol,florfenicol and its main metabolite,florfenicolamine,and should have a relatively low limit of detection（LOD）. [Method] The milk was precipitated with trichloroacetic acid to remove proteins,extracted with ammoniated ethyl acetate,purified by MCX solid-phase extraction column,and re-solubilized in a methanol-water solution,separated on a Waters ACQUITY UPLC HSS T3 column（2.1 mm×100 mm,1.8 μm）,and eluted with a gradient of 25% methanol（channel A）and 75% water[containing 100 μL of ammoniated methanol（5%）in 200 mL water,channel B]. Mass spectrometry analysis was performed using multiple reaction monitoring（MRM）,and quantification was determined by external standard method. [Result] This method could complete the detection of 4 amphenicol compounds within 5 minutes. The recovery rates of the 4 amphenicol compounds at the added levels of 0.3,0.6,1.5 μg/kg was 77.3% to 106.4%,with the relative standard deviation ranging from 1.6% to 11.8%（n=6）. The LOD of the method was 0.1 μg/kg and the limit of quantification（LOQ）was 0.3 μg/kg. [Conclusion] This method was comprehensive,rapid,highly accurate,highly sensitive and stable,making it suitable for the detection of four amphenicol antibiotic residues in milk.