| 引用本文: | 冯炎林,洪滟,田伟强.UPLC-MS/MS测定大鼠舌下静脉注射阿西替尼的血药浓度及其药动学研究[J].中国现代应用药学,2017,34(9):1304-1308. |
| FENG Yanlin,HONG Yan,TIAN Weiqiang.Study on Plasma Concentration and Pharmacokinetics of Axitinib After Intravenous Administration in Rats by UPLC-MS/MS[J].Chin J Mod Appl Pharm(中国现代应用药学),2017,34(9):1304-1308. |
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| 摘要: |
| 目的 建立UPLC-MS/MS对舌下静脉注射大鼠血浆中阿西替血药浓度的检测方法，并进行其药动学研究。方法 乙腈沉淀法处理样品，以伊马替尼为内标，Waters Acquity BEH C18色谱柱（2.1 mm×100 mm，1.7 μm），流动相为0.1%甲酸水和乙腈。流速为0.3 mL·min-1，柱温35℃。质谱条件为电喷雾电离源（ESI），检测方式为正离子电离、多离子反应监测（MRM）检测。结果 阿西替尼血药浓度在0.1~100 ng·mL-1内线性关系良好（r=0.999 6），定量下限为0.1 ng·mL-1。日内、日间精密度RSD<5.56%，提取回收率>87.87%。大鼠血浆中的阿西替尼在室温、4℃，-80℃，12 h后以及反复冻融3次后均有良好的稳定性，且不存在基质效应。结论 建立的测定阿西替尼血药浓度的方法准确、简单、快速，可以为阿西替尼的临床研究提供实验参考和依据。 |
| 关键词: 阿西替尼 超高效液相色谱串联质谱法 静脉给药 |
| DOI：10.13748/j.cnki.issn1007-7693.2017.09.019 |
| 分类号:R917.101 |
| 基金项目: |
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| Study on Plasma Concentration and Pharmacokinetics of Axitinib After Intravenous Administration in Rats by UPLC-MS/MS |
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FENG Yanlin, HONG Yan, TIAN Weiqiang
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Department of Phmarcy, the Fifth Affiliated Hospital of Wenzhou Medical University, Lishui Municipal Central Hospital, Lishui 323000, China
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| Abstract: |
| OBJECTIVE To develop a ultra high-performance liquid chromatography-tandem mass spectrometry separation method(UPLC-MS/MS) for the pharmacokinetic study of Axitinib after intravenous administration. METHODS Plasma samples were treated by acetonitrile precipitation. The effective UPLC-MS/MS separation of the examined compounds was applied on an Acquity BEH C18 column (2.1 mm×50 mm, 1.7 μm) column with a gradient mobile phase system consisting of 0.1% formic acid in water and acetonitrile. The analysis was performed with a flow rate of 0.3 mL·min-1. An electrospray ionization (ESI) was used to detect in a positive ion mode. The scanning mode was MRM. RESULTS The assay was validated over concentration ranges of 0.1-100 ng·mL-1, with a lower limit of quantification (LLOQ) of 0.1 ng·mL-1. Intra-and inter-assay precision values for replicate quality control samples were within 5.56%. Assay recoveries of Axitinib was higher than 87.87%. Axitinib were stable in rat plasma for at least 24 h at room temperature, 30 days at 4℃ and -20℃, and following at least three freeze-thaw cycles. Furthermore, no notable matrix effect was observed for Axitinib. CONCLUSION The accurate and simple method developed can be provided the basis and applied to clinical pharmacokinetic study. |
| Key words: Axitinib UPLC-MS/MS intravenous administration |
