中国科学院机构知识库网格
Chinese Academy of Sciences Institutional Repositories Grid
On-cartridge derivatization coupled with solid-phase extraction for the ultra-sensitive determination of minodronic acid in human plasma by LC-MS/MS method

文献类型:期刊论文

作者Yang, Yong; Liu, Cai; Zhang, Yifan; Zhou, Lei; Zhong, Dafang; Chen, Xiaoyan
刊名JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
出版日期2015-10-10
卷号114页码:408-415
关键词Minodronic acid Derivatization Trimethylsilyldiazomethane Bisphosphonate LC-MS/MS
ISSN号0731-7085
DOI10.1016/j.jpba.2015.05.038
文献子类Article
英文摘要Minodronic acid (MA) is a third-generation bisphosphonate (BP). Its high potency allows lower doses to be administered in clinical settings compared with other BPs, which results in extremely low systemic exposure. Therefore, it is essential to develop an ultra-sensitive bioassay for pharmacokinetics studies of MA. In this work, we used on-cartridge derivatization of MA with trimethylsilyldiazomethane to extract MA from plasma samples and improve its LC-MS/MS behavior. The reaction produced a known derivative, tetramethylated MA, and a novel derivative, pentamethylated MA (PMMA). PMMA exhibited a better signal-to-noise ratio, and was monitored for the quantification of MA. However, the derivatization yield of d4-PMMA was much lower and more variable than that of PMMA, which decreased the effectiveness of its correction function as an internal standard. Therefore, a two-cycle derivatization approach was introduced to increase its yield and improve the reproducibility. The calibration curves of MA showed good linearity over the range of 10.0-1000 pg/mL. A lower limit of quantification of 10.0 pg/mL was achieved with acceptable precision (<10.5%) and accuracy (5.0%). The intra- and inter-batch precision of quality control samples was <9.5%, and the accuracy ranged from -2.8% to 0.6%. The stability results showed that MA was stable in human plasma for 6 h at room temperature (25 degrees C), for 115 days at -20 degrees C, during three freeze/thaw cycles (from -20 degrees C to 25 degrees C), and in post-preparative samples for 24h at 4 degrees C. The method was successfully used to characterize the pharmacokinetic profile of MA following an oral dose of 1.0 mg MA hydrate to healthy volunteers (n = 12). The proposed derivatization procedure was also extended to measure other BPs (risedronic acid and zoledronic acid) in human plasma at low pg/mL. (C) 2015 Elsevier B.V. All rights reserved.
WOS关键词PERFORMANCE LIQUID-CHROMATOGRAPHY ; MASS-SPECTROMETRY ; FLUORESCENCE DETECTION ; ZOLEDRONIC ACID ; HUMAN URINE ; BISPHOSPHONATES ; BONE ; RISEDRONATE ; TRIMETHYLSILYLDIAZOMETHANE
WOS研究方向Chemistry ; Pharmacology & Pharmacy
语种英语
WOS记录号WOS:000360780700053
出版者ELSEVIER SCIENCE BV
源URL[http://119.78.100.183/handle/2S10ELR8/276365]  
专题上海药物代谢研究中心
通讯作者Chen, Xiaoyan
作者单位Chinese Acad Sci, Shanghai Inst Mat Med, Ctr Drug Metab & Pharmacokinet, Shanghai 201203, Peoples R China
推荐引用方式
GB/T 7714
Yang, Yong,Liu, Cai,Zhang, Yifan,et al. On-cartridge derivatization coupled with solid-phase extraction for the ultra-sensitive determination of minodronic acid in human plasma by LC-MS/MS method[J]. JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS,2015,114:408-415.
APA Yang, Yong,Liu, Cai,Zhang, Yifan,Zhou, Lei,Zhong, Dafang,&Chen, Xiaoyan.(2015).On-cartridge derivatization coupled with solid-phase extraction for the ultra-sensitive determination of minodronic acid in human plasma by LC-MS/MS method.JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS,114,408-415.
MLA Yang, Yong,et al."On-cartridge derivatization coupled with solid-phase extraction for the ultra-sensitive determination of minodronic acid in human plasma by LC-MS/MS method".JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS 114(2015):408-415.

入库方式: OAI收割

来源:上海药物研究所

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