色谱2012，Vol.30Issue(5)：445-451,7.DOI:10.3724/SP.J.1123.2011.11036
超高效液相色谱-串联质谱法同时测定全血中青霉素G及其主要代谢产物
Simultaneous determination of penicillin G and its major metabolites in blood using ultra performance liquid chromatography-tandem mass spectrometry
摘要
Abstract
A fast method for the quantitative determination of penicillin G (PEN G) , penicilloic acid and penilloic acid in blood with ultra performance liquid chromatography-electrospray tandem mass spectrometry was developed. A simple deproteinization of the blood was used with a mixed solution of acetonitrile and water (4:1, v/v) as extraction solvent. The blood extract was directly injected onto an LC column. The chromatographic separation of the components was performed on a BEH C18 column (50 mm x2. 1 mm, 1. 7祄) using acetonitrile and water containing 0. 1 % formic acid. The mass spectrometer was operated in positive electrospray ion mode. Finally, the analysis was carried out with multiple reaction monitoring (MRM) mode. The limits of detection (LODs) for these three compounds were in the range of 0. 1 to 2. 0 ng/mL and the limits of quantification (LOQs) in the range of 0. 5 to 5. 0 ng/mL. Within the linear range, the correlation coefficients (r) of PEN G and its metabolites were all more than 0. 997 4. Accuracies for these targeted compounds were ranged from 92. 3% to 105. 5%, and the within-day precisions were less than 10%. The stabilities of the components were evaluated in the temperature range from 18 to - 80?, and the mass concentration of penicillin G was decreased significantly with the extensions of storage temperature and storage time. Biological samples of the rats medicated with PEN G were analyzed using the developed method. The results show that PEN G can just be detected at 0. 5 h after administration. However, the detection time limitation of penicilloic acid can be extended to 36 h. The established method has been further expanded for the applicability of forensic identification, and has a reference value for the detection of penicillin G residue in food.关键词
超高效液相色谱-串联质谱/青霉素G/代谢产物/全血Key words
ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) / penicillin G/ metabolites/ blood分类
化学化工引用本文复制引用
陈聪,严慧,沈保华,卓先义..超高效液相色谱-串联质谱法同时测定全血中青霉素G及其主要代谢产物[J].色谱,2012,30(5):445-451,7.基金项目
上海市法医学重点实验室项目(11DZ2271500,2009-2). （11DZ2271500,2009-2）
