法医学杂志

法医学杂志 ›› 2011, Vol. 27 ›› Issue (1): 25-29.DOI: 10.3969/j.issn.1004-5619.2011.01.007

• 论著 • 上一篇    下一篇

超高效液相色谱-串联质谱法同时测定尿液中16种抗生素

陈  聪1，2，严  慧2，沈保华2，卓先义2   

  1. （1. 复旦大学 上海医学院法医学系，上海 200032； 2. 司法部司法鉴定科学技术研究所 上海市法医学重点实验室，上海 200063）
  • 发布日期:2011-02-25 出版日期:2011-02-28
  • 通讯作者: 通信作者：卓先义，研究员，硕士研究生导师，主要从事毒物化学研究；E-mail：zhuoxy@ssfjd.cn
  • 作者简介:陈聪（1984—），男，浙江绍兴人，硕士研究生，主要从事毒物化学研究；E-mail：xiangfei218516@163.com

Simultaneous Determination of Sixteen Antibiotics in Human Urine with Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

CHEN CONG1,2, YAN HUI2, SHEN BAO-HUA2, ZHUO XIAN-YI2   

  1. （1. Department of Forensic Medicine, Shanghai Medical College of Fudan University, Shanghai 200032, China; 2. Shanghai Key Laboratory of Forensic Medicine, Institute of Forensic Science, Ministry of Justice, P.R.China, Shanghai 200063, China）
  • Online:2011-02-25 Published:2011-02-28

被引次数

7

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0.05~10.0 ng/mL，定量限（LOQ）为0.25~20.0 ng/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。

关键词: 法医毒理学, 抗生素, 尿, 超高效液相色谱-串联质谱法

Abstract: 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 0.05-10.0 ng/mL and the limits of quantification（LOQ） in the range of 0.25-20.0 ng/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.

Key words: forensic toxicology, antibiotics, urine, ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）

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