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![]() ![]() ![]() |
刊名 | JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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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 |
DOI | 10.1016/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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