化学
色谱法
醋酸铵
醋酸
选择性反应监测
甲醇
质谱法
药代动力学
串联质谱法
液相色谱-质谱法
洗脱
小猎犬
高效液相色谱法
医学
内科学
有机化学
生物化学
作者
Shailendra Shakya,He Zhu,Li Ding,Xiao Lang Du,Xie Min Qi,Xiao Yang,Zhong Lin Yang
摘要
ABSTRACT A sensitive and rapid liquid chromatography–tandem mass spectrometry (LC‐MS/MS) method has been developed and validated for the determination of asperosaponin VI in beagle dog plasma using glycyrrhizic acid as the internal standard (IS). Plasma samples were simply pretreated with methanol for deproteinization. Chromatographic separation was performed on a Hedera ODS‐2 column using mobile phase of methanol–10 m m ammonium acetate buffer solution containing 0.05% acetic acid (71:29, v/v) at a flow rate of 0.38 mL/min. Asperosaponin VI and the IS were eluted at 2.8 and 1.9 min, respectively, ionized in negative ion mode, and then detected by multiple reaction monitoring. The detection used the transitions of the deprotonated molecules at m / z 927.5 → 603.4 for asperosaponin VI and m / z 821.4 → 645.4 for glycyrrhizic acid (IS). The assay was linear over the concentration range of 0.15–700 ng/mL and was successfully applied to a pilot pharmacokinetic study in beagle dogs. Copyright © 2011 John Wiley & Sons, Ltd.
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