Shakya Shailendra, Zhu He, Ding Li, Du Xiao Lang, Qi Xie Min, Yang Xiao Lin, Yang Zhong Lin
Department of Pharmaceutical Analysis, China Pharmaceutical University, 24 Tongjiaxiang, Nanjing, China.
Biomed Chromatogr. 2012 Jan;26(1):109-14. doi: 10.1002/bmc.1634. Epub 2011 Apr 5.
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 mm 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.
已建立并验证了一种灵敏且快速的液相色谱 - 串联质谱（LC-MS/MS）方法，以甘草酸作为内标（IS）测定比格犬血浆中的asperosaponin VI。血浆样品只需用甲醇进行简单的蛋白沉淀预处理。采用Hedera ODS - 2柱进行色谱分离，流动相为甲醇 - 含0.05%乙酸的10 mM乙酸铵缓冲溶液（71:29，v/v），流速为0.38 mL/min。Asperosaponin VI和内标分别在2.8分钟和1.9分钟洗脱，在负离子模式下电离，然后通过多反应监测进行检测。检测采用了asperosaponin VI的去质子化分子在m/z 927.5 → 603.4的跃迁以及甘草酸（内标）在m/z 821.4 → 645.4的跃迁。该测定法在0.15 - 700 ng/mL的浓度范围内呈线性，并成功应用于比格犬的初步药代动力学研究。
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