Chen Cong, Yan Hui, Shen Bao-hua, Zhuo Xian-yi
Department of Forensic Medicine, Shanghai Medical College of Fudan University, Shanghai 200032, China.
Fa Yi Xue Za Zhi. 2011 Feb;27(1):25-9.
To develop a method for simultaneous determination of sixteen antibiotics in human urine by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS).
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.
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%.
The developed method is sensitive, specific and appropriate for the analysis of antibiotics in forensic toxicology and therapeutic drugs monitoring.
建立超高效液相色谱-串联质谱法(UPLC-MS/MS)同时测定人尿液中16种抗生素的方法。
以哌拉西林为内标,尿液样品中的目标抗生素经Oasis HLB固相萃取(SPE)柱富集纯化,然后在ZORBAX SB-C18柱上以0.1%甲酸水和乙腈为流动相进行梯度洗脱分离,最后采用多反应监测(MRM)模式进行分析。
这16种抗生素的检测限(LOD)在0.05-10.0 ng/mL范围内,定量限(LOQ)在0.25-20.0 ng/mL范围内。在相关线性范围内,16种抗生素的相关系数(r)均大于0.995。这些抗生素的准确度在82.0%-119.3%之间,日内精密度小于13.9%。
所建立的方法灵敏、特异,适用于法医毒理学和治疗药物监测中抗生素的分析。