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采用正负离子切换模式的LC-ESI-MS/MS法测定大鼠灌胃给药后京尼平苷的血浆浓度(英文)
引用本文:邓志鹏,范惠霞,仲浩,崔淑香,姚庆强. 采用正负离子切换模式的LC-ESI-MS/MS法测定大鼠灌胃给药后京尼平苷的血浆浓度(英文)[J]. 中国药学, 2013, 22(3): 234-238. DOI: 10.5246/jcps.2013.03.033
作者姓名:邓志鹏  范惠霞  仲浩  崔淑香  姚庆强
作者单位:山东省医学科学院药物研究所
基金项目:Laboratory for Rare Disease of Shandong Province
摘    要:建立了一种快速、专属性强的液相色谱-串联质谱方法(LC-MS/MS)测定中药栀子的主要活性成分–京尼平苷的大鼠血药浓度去评价其临床前药动学特征。京尼平苷血浆样品经沉淀蛋白后,采用DiamonsilC18色谱柱进行分析,采用流动相10mM醋酸铵–甲醇(20:80,v/v),流速0.6mL/min。样品测定采用"Truncated"多反应检测模式,采用正离子m/z411→411测定京尼平苷,采用负离子m/z415→295测定内标葛根素。线性浓度范围为10.0–5000ng/mL,最低定量下限为10.0ng/mL,样品提取回收率范围为84.8%–90.5%。该确证方法成功应用于大鼠灌胃(给药剂量200mg/kg)给予京尼平苷后的药动学研究。

关 键 词:LC-MS/MS  蛋白沉淀  大鼠血浆  药动学  京尼平苷
收稿时间:2012-08-29

Development of a method for the quantitative determination of geniposide in rat plasma by ......
Zhipeng Deng, Huixia Fan, Hao Zhong, Shuxiang Cui, Qingqiang Yao. Development of a method for the quantitative determination of geniposide in rat plasma by ......[J]. Journal of Chinese Pharmaceutical Sciences, 2013, 22(3): 234-238. DOI: 10.5246/jcps.2013.03.033
Authors:Zhipeng Deng   Huixia Fan   Hao Zhong   Shuxiang Cui   Qingqiang Yao
Affiliation:* Institute of Materia Medica, Shandong Academy of Medical Sciences, Jinan 250062, China
Abstract:Geniposide is a major bioactive constituent isolated from Gardenia jasminoides Ellis. To evaluate the pharmacokinetics of geniposide in pre-clinical studies, a rapid and specific liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated. After simple protein precipitation, geniposide was analyzed on a Diamonsil® C18 column with a mobile phase of 10 mM ammonium acetate and methanol (20:80, v/v) at a flow rate of 0.6 mL/min. Detection was performed in "Truncated" multiple-reaction monitoring (MRM) mode with positive electrospray ionization (ESI) at m/z 411→411 for geniposide, and MRM mode with negative ESI ionization at m/z 415→295 for puerarin (internal standard, IS). Linearity was established in the concentration range from 10.0 to 5000 ng/mL. The extraction recoveries ranged from 84.8% to 90.5% at concentrations of 10.0, 500 and 4.5×103 ng/mL. The lower limit of quantification (LLOQ) was 10.0 ng/mL with 50 µL plasma. The validated method was successfully applied to the pharmacokinetic study of geniposide in rats at a dose of 200 mg/kg by oral administration.
Keywords:LC-MS/MS   Protein precipitation   Rat plasma   Pharmacokinetics   Geniposide  
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