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建立了鱼类中糖肽类抗生素万古霉素和去甲万古霉素残留量的双固相萃取/高效液相色谱-串联质谱(LC-MS/MS)检测方法.样品经0.1％甲酸水-乙腈(7:3,V/V)混合溶液提取,乙腈饱和的正己烷去脂,固相萃取柱C18及PCX净化,在多反应监测(MRM)正离子模式下进行检测,使用双去氯万古霉素作为内标物,内标法定量.实验结果表明,万古霉素和去甲万古霉素在2～250 ng/mL范围内呈良好的线性关系,相关系数(r2)大于0.99.在5,25,100μg/kg 3个添加水平下平均回收率为92.8％ ～96.5％,相对标准偏差为4.5％ ～7.0％.方法检出限(LOD)为2.0μg/kg,定量限(LOQ)为5.0μg/kg.方法适用于鱼类中糖肽类抗生素万古霉素和去甲万古霉素残留量的测定.“,”A new method for the determination of glycopeptide antibiotics residues including vancomycin and norvancomycin in fish by high performance liquid chromatography-mass spectrometry ( LC-MS/MS ) coupled with dual solid-phase extraction was established. Samples were extracted with 0. 1％ formic acid-acetonitrile solution (7:3, V/V), defatted by n-hexane saturated with acetonitrile, purified by SPE C18 and PCX column, analyzed under the multiple reaction monitoring (MRM) mode, and quantified by Dedichloro vancomycin as internal standard. The results showed good linearity in the range of 2～250 ng/mL, and the correlation coefficient ( r2 ) was greater than 0. 99. At the spiked levels of 5, 25 and 100 μg/kg, the average recoveries were in the range of 92. 8％ ～96. 5％ with the relative standard deviations from 4. 5％ to 7. 0％ . The limit of detection (LOD) of this method was 2. 0μg/kg, and limit of quantitation (LOQ) was 5. 0 μg/kg. The results indicated that this method could be used for the simultaneous determination of Vancomycin and Norvancomycin residues in fish.