Analysis of Theophylline and Its Metabolites in Human Urine by Precolumn Derivatization Coupled with Liquid Chromatography Tandem Mass Spectrometry
文献类型:期刊论文
作者 | Yao Zhihong4; Wu Xiaomeng2; Sun Lu3; Zhong Dafang1![]() |
刊名 | Journal of Instrumental Analysis
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出版日期 | 2015 |
卷号 | 34期号:7页码:795-801 |
关键词 | theophylline in vivo metabolites LC - MS~n precolumn derivatization |
ISSN号 | 1004-4957 |
其他题名 | 柱前衍生化结合LC-MS~n分析人尿中茶碱及其代谢物 |
文献子类 | Article |
英文摘要 | A solid phase extraction and precolumn chemical derivatization technique coupled with liquid chromatography - electrospray ionization /mass spectrometric(LC - ESI /MS~n) method was developed for the analysis of theophylline and its metabolites in human urine after oral administration of theophylline tablets to discover its metabolism pathway in vivo. The mass spectral fragmentation behaviors of theophylline,metabolites and their derivatives were also discussed. Human urine between 0 hour and 6 hour was collected immediately after administration of theophylline tablets. Then the urine samples were pretreated by solid phase extraction through a Bond Elute C_(18) column. Methanol part was collected to be dried by N_2 at 50 ℃,and then subjected to derivatization with N,N-dimethyl ethylamine chloride. The separation of urine samples was achieved on a Shimpack C_(18) column with methanol - water - formic acid(20 ∶ 80 ∶ 1) as mobile phase,and the detection was fulfilled with electro spray ionization(ESI) in positive mode. Through this method,theophylline and four metabolites(1-methyl uric acid,1,3-dimethyl uric acid,1-methyl-N-acetyl derivative and 3-methyl xan thine) were identified or tentatively identified,in which one of these metabolites was firstly recovered in theophylline. Under positive mode,theophylline and its metabolites always lost 18 u,28 u or 57 u fragments in MS~2 spectrum and their derivatives lost 45 u fragments regularly in MS~2 spectrum. Through the comparison with the underivatized urine samples,the samples derivatized were found to be able to enhance the sensitivity of theophylline,1-methyl uric acid and 3-methyl xanthine in mass spectrometry. This method replenished the metabolite file of theophylline in human,and provided a new approach for the identification of theophylline,metabolites and their structural analogues with low concentration in biosamples. |
WOS研究方向 | Chemistry (provided by Clarivate Analytics) |
语种 | 中文 |
CSCD记录号 | CSCD:5483487 |
源URL | [http://119.78.100.183/handle/2S10ELR8/269276] ![]() |
专题 | 上海药物代谢研究中心 |
作者单位 | 1.Shanghai Institute of Materia Medica,Chinese Academy of Sciences, Shanghai 201203, China. 2.College of Pharmacy,Jinan University, Guangzhou, Guangdong 510632, China.; 3.College of Pharmacy,Shenyang Pharmaceutical University, Shenyang, Liaoning 110016, China.; 4.Guangdong Province Key Laboratory of Pharmacodynamic Consitituents of Traditional Chinese Medicine and New Drug Research, Guangzhou, Guangdong 510632, China.; |
推荐引用方式 GB/T 7714 | Yao Zhihong,Wu Xiaomeng,Sun Lu,et al. Analysis of Theophylline and Its Metabolites in Human Urine by Precolumn Derivatization Coupled with Liquid Chromatography Tandem Mass Spectrometry[J]. Journal of Instrumental Analysis,2015,34(7):795-801. |
APA | Yao Zhihong,Wu Xiaomeng,Sun Lu,&Zhong Dafang.(2015).Analysis of Theophylline and Its Metabolites in Human Urine by Precolumn Derivatization Coupled with Liquid Chromatography Tandem Mass Spectrometry.Journal of Instrumental Analysis,34(7),795-801. |
MLA | Yao Zhihong,et al."Analysis of Theophylline and Its Metabolites in Human Urine by Precolumn Derivatization Coupled with Liquid Chromatography Tandem Mass Spectrometry".Journal of Instrumental Analysis 34.7(2015):795-801. |
入库方式: OAI收割
来源:上海药物研究所
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