Development and validation of an HPLC-MS/MS method to determine clopidogrel in human plasma
文献类型：期刊论文
| 作者 | Liu, Gangyi1; Dong, Chunxia1; Shen, Weiwei1; Lu, Xiaopei1; Zhang, Mengqi1; Gui, Yuzhou2; Zhou, Qinyi1; Yu, Chen1 |
| 刊名 | ACTA PHARMACEUTICA SINICA B
 |
| 出版日期 | 2016-01 |
| 卷号 | 6期号:1页码:55-63 |
| 关键词 | Clopidogrel Online-SPE LC MS/MS Back-conversion Bioequivalence Deuterated analogue Real samples stability FDA guidelines |
| ISSN号 | 2211-3835 |
| DOI | 10.1016/j.apsb.2015.11.001 |
| 文献子类 | Article |
| 英文摘要 | A quantitative method for clopidogrel using online-SPE tandem LC-MS/MS was developed and fully validated according to the well-established FDA guidelines. The method achieves adequate sensitivity for pharmacokinetic studies, with lower limit of quantifications (LLOQs) as low as 10 pg/mL. Chromatographic separations were performed on reversed phase columns Kromasil Eternity-2.5-C18-UHPLC for both methods. Positive electrospray ionization in multiple reaction monitoring (MRM) mode was employed for signal detection and a deuterated analogue (clopidogrel-d(4)) was used as internal standard (IS). Adjustments in sample preparation, including introduction of an online-SPE system proved to be the most effective method to solve the analyte back-conversion in clinical samples. Pooled clinical samples (two levels) were prepared and successfully used as real-sample quality control (QC) in the validation of back-conversion testing under different conditions. The result showed that the real samples were stable in room temperature for 24 h. Linearity, precision, extraction recovery, matrix effect on spiked QC samples and stability tests on both spiked QCs and real sample QCs stored in different conditions met the acceptance criteria. This online-SPE method was successfully applied to a bioequivalence study of 75 mg single dose clopidogrel tablets in 48 healthy male subjects. (C) 2016 Chinese Pharmaceutical Association and Institute of Materia Medica, Chinese Academy of Medical Sciences. Production and hosting by Elsevier B.V. |
| WOS关键词 | OPEN-LABEL ; CORONARY ; BIOEQUIVALENCE ; METABOLITE ; BISULFATE ; CROSSOVER ; THERAPY |
| WOS研究方向 | Pharmacology & Pharmacy |
| 语种 | 英语 |
| CSCD记录号 | CSCD:5625138 |
| WOS记录号 | WOS:000371987700006 |
| 出版者 | INST MATERIA MEDICA, CHINESE ACAD MEDICAL SCIENCES |
| 源URL | [http://119.78.100.183/handle/2S10ELR8/276239]  |
| 专题 | 新药研究国家重点实验室 中科院受体结构与功能重点实验室 |
| 通讯作者 | Yu, Chen |
| 作者单位 | 1.Chinese Acad Sci, Shanghai Xuhui Cent Hosp, Shanghai Clin Ctr, Cent Lab, Shanghai 200031, Peoples R China; 2.Chinese Acad Sci, Shanghai Inst Mat Med, State Key Lab Drug Res, Shanghai 200233, Peoples R China |
| 推荐引用方式 GB/T 7714 | Liu, Gangyi,Dong, Chunxia,Shen, Weiwei,et al. Development and validation of an HPLC-MS/MS method to determine clopidogrel in human plasma[J]. ACTA PHARMACEUTICA SINICA B,2016,6(1):55-63. |
| APA | Liu, Gangyi.,Dong, Chunxia.,Shen, Weiwei.,Lu, Xiaopei.,Zhang, Mengqi.,...&Yu, Chen.(2016).Development and validation of an HPLC-MS/MS method to determine clopidogrel in human plasma.ACTA PHARMACEUTICA SINICA B,6(1),55-63. |
| MLA | Liu, Gangyi,et al."Development and validation of an HPLC-MS/MS method to determine clopidogrel in human plasma".ACTA PHARMACEUTICA SINICA B 6.1(2016):55-63. |
入库方式： OAI收割
来源：上海药物研究所
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