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学科主题: 临床医学
题名:
Development and validation of a rapid and sensitive liquid chromatography-tandem mass spectrometry method for benvitimod quantification in human plasma
作者: Zhao, Libo1; Zhu, Baoying2; Chen, Xin1; Chen, Genghui3; Chen, Haibo4; Li, Yuzhen1; Jing, Shan1; Fang, Yi1
关键词: Benvitimod ; LC/ESI/MS/MS ; Human plasma ; Pharmacokinetics
刊名: JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
发表日期: 2012-02-15
DOI: 10.1016/j.jchromb.2011.12.026
卷: 885, 页:160-165
收录类别: SCI
文章类型: Article
WOS标题词: Science & Technology
类目[WOS]: Biochemical Research Methods ; Chemistry, Analytical
研究领域[WOS]: Biochemistry & Molecular Biology ; Chemistry
关键词[WOS]: PERFORMANCE
英文摘要:

Benvitimod is a newly synthesized non-steroid small molecule being developed as a candidate drug for the treatment of inflammatory skin diseases. Here a rapid, sensitive and specific high performance liquid chromatography-tandem mass spectrometry (LC/ESI/MS/MS) method was developed for the determination of benvitimod in human plasma. The samples were alkalified with disodium tetraborate firstly, and then extracted by methyl tert-butyl ether. Fluorophenyl-benvitimod was used as internal standard (IS.). Chromatographic separation was performed on an Ultra C-18 column (150 mm x 2.1 mm, 5.0 mu m). The mixed mobile phase delivered at 300 mu l/min was CH3CN/H2O, 76.65:23.35 (v/v), containing 0.2 mmol/L NH4COOH. Detection and quantitation was performed by electrospray ionization (ESI) and multiple reaction monitoring (MRM) in the negative ion mode. The most intense [M-H](-) MRM transition of benvitimod at m/z 253.1 -> 211.0 was used for benvitimod quantitation and the transition at m/z 270.9 -> 229.2 was used to monitor I.S. The calibration curve was linear within the concentration range of 0.1-10.0 ng/mL (r > 0.99). The lower limit of quantification (LLOQ) was 0.1 ng/mL. The extraction recovery was above 80%. The accuracy expressed as relative error (RE) was less than 1.03%. The intra- and inter-day precisions were less than 11.81%. The freeze-thaw stability was also investigated and it was found that both benvitimod and the 1.5. were quite stable. This method is especially useful for the pharmacokinetic study of benvitimod. (C) 2012 Elsevier B.V. All rights reserved.

语种: 英语
WOS记录号: WOS:000301563400021
Citation statistics:
内容类型: 期刊论文
URI标识: http://ir.bjmu.edu.cn/handle/400002259/51027
Appears in Collections:北京大学第二临床医学院_药剂科_期刊论文

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作者单位: 1.Peking Univ Peoples Hosp, Dept Pharm, Beijing 100044, Peoples R China
2.Guiyang Med Coll, Guiyang 550004, Peoples R China
3.Celestial Pharmaceut Co Ltd, Shenzhen 518057, Peoples R China
4.Xuzhou Med Coll, Xuzhou 221004, Peoples R China

Recommended Citation:
Zhao, Libo,Zhu, Baoying,Chen, Xin,et al. Development and validation of a rapid and sensitive liquid chromatography-tandem mass spectrometry method for benvitimod quantification in human plasma[J]. JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES,2012,885:160-165.
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