超高效液相色谱-串联质谱法同时测定尿液中16种抗生素

摘要

目的 建立同时分析尿液中16种抗生素的超高效液相色谱-串联质谱(UPLC-MS、MS)方法.方法 以哌拉西林为内标.尿样中的目标化合物经Oasis HLB固相萃取柱富集、纯化,利用ZORBAX SB-C18色谱柱,以0.1%的甲酸溶液-乙腈为流动相经梯度洗脱分离,采用多反应监测(MRM)模式进行分析.结果各化合物的最低检出限(LOD)为0.05～10.0ng/mL,定量限(LOQ)为0.25～20.0ng/mL.在相应线性范围内,16种抗生素的相关系数(r)均大于0.995.方法 准确度为82.0%～119.3%,日内精密度均小于13.9%.结论 所建方法灵敏度高、选择性好,可用于法医毒物分析和临床药物监测中的抗生素测定.%Objective To develop a method for simultaneous determination of sixteen antibiotics in human urine by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods With Piperacillin as an internal standard, the target antibiotics in urine samples were enriched and purified by Oasis HLB solid phase extraction(SPE) cartridges, then separated in a ZORBAX SB-C18 column with a gradient elution of mobile phase of 0.1％ formic acid water and acetonitrile, finally analyzed with multiple reaction monitoring (MRM) mode. Results The limits of detection (LOD) for these sixteen antibiotics were in the range of 0.05-10.0ng/mL and the limits of quantification (LOQ) in the range of 0.25-20.0ng/mL.Within the related linear range, the related coefficient (r) of sixteen antibiotics were all more than 0.995.Accuracies for these antibiotics were ranged from 82.0％-119.3％, the within-day precision were less than 13.9％. Conclusion The developed method is sensitive, specific and appropriate for the analysis of antibiotics in forensic toxicology and therapeutic drugs monitoring.