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| LC－MS/MS法测定升麻葛根汤颗粒在犬体内的药代动力学研究 |
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常梦春1,2, 刘静静1,2, 刘勃缨1,2, 任静1,2, 张丽娜1,2, 李佳玮1,2, 刘志东1,2
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1.天津中医药大学, 现代中药发现与制剂技术教育部工程中心, 天津 300193;2.天津中医药大学, 天津市现代中药重点实验室-省部共建国家重点实验室培育基地, 天津 300193
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| 摘要: |
| [目的] 建立液相色谱-质谱联用（LC－MS/MS）的方法测定犬灌胃给药升麻葛根汤颗粒后葛根素、芍药苷、异阿魏酸的药代动力学。[方法] 采用Waters ACQUITY UPLC® BEH C18柱（2.1 mm×50 mm，1.7 μm），流动相：0.05%甲酸水（A）-乙腈（B）梯度洗脱；流速：0.2 mL/min；柱温：25℃；进样量：5 μL。以甲苯磺丁脲为内标，采用电喷雾离子源（ESI离子源），在负离子检测方式下进行多反应离子检测（MRM），检测离子对分别为m/z 415.2→294.9（葛根素）、m/z 525.0→449.0（芍药苷）、m/z 193.05→133.9（异阿魏酸）、m/z 269.09→169.9（甲苯磺丁脲，内标）。[结果] 葛根素、芍药苷、异阿魏酸在10~4 000 ng/mL范围内线性关系良好。血浆中内源性物质不干扰测定，方法回收率、基质效应、精密度、准确度和稳定性均符合生物样品的测定要求。[结论] 该方法准确度强，专属性好，灵敏度高，可用于检测葛根素、芍药苷、异阿魏酸的药代动力学。 |
| 关键词: 升麻葛根汤颗粒 LC－MS/MS 犬 药代动力学 |
| DOI：10.11656/j.issn.1673-9043.2019.01.18 |
| 分类号:R285.5 |
| 基金项目:天津市自然科学基金（15PTCYSY00030，16ZXHLGX00170）。 |
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| Study on the pharmacokinetics of Shengma Gegen decoction granule in beagle dogs by LC-MS/MS |
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CHANG Mengchun1,2, LIU Jingjing1,2, LIU Boying1,2, REN jing1,2, ZHANG Lina1,2, LI Jiawei1,2, LIU Zhidong1,2
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1.Engineering Research Center of Modern Chinese Medicine Discovery and Preparation Technique, Ministry of Education, Tianjin University of Traditional Chinese Medicine, Tianjin 300193, China;2.Tianjin State Key Laboratory of Modern Chinese Medicine, Tianjin 300193, China
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| Abstract: |
| [Objective] LC-MS/MS was developed for the determination of the pharmacokinetics of puerarin,paeoniflorin and isoferulic acid in dogs after oral Shengma Gegen decoction granule.[Methods] The column of Waters ACQUITY UPLC® BEH C18(1.7 μm,2.1 mm×50 mm)and a mixture of 0.05% formic acid water solution (A)-acetonitrile(B) as the mobile phase at the flow-rate of 0.2 mL/min,the column temperature was 25℃ and the injection volume was 5 μL.Tolbutamide was used as the internal standard,detection was by negative ion electrospray ionization (ESI) mass spectrometry with multiple-reaction monitoring (MRM). Detection of ion pairs respectively are m/z 415.2→294.9 for puerarin,m/z 525.0→449.0 for paeoniflorin,m/z 193.05→133.9 for isoferulic acid,m/z 269.09→169.9 for tolbutamide.[Results] For the puerarin,paeoniflorin and isoferulic acid,the linear calibration curves were obtained over the concentration range 10~4 000 ng/mL.Endogenous substances in the plasma do not interfere with the determination,the recovery rate,matrix effect,precision,accuracy and stability of the method are in accordance with the requirements of biological samples.[Conclusion] The method has the advantages of strong accuracy,good specificity and high sensitivity,and can be used to detect the pharmacokinetics of puerarin,paeoniflorin and isoferulic acid. |
| Key words: Shengma Gegen decoction granule LC-MS/MS beagle dogs pharmacokinetics |
