化学
色谱法
蛋白质沉淀
药代动力学
电喷雾电离
串联质谱法
选择性反应监测
质谱法
三七
液相色谱-质谱法
分析物
电喷雾
检出限
基质(化学分析)
作者
Zhengcai Ju,Chunyong He,Jia Li,Li Yang,Zhengtao Wang
摘要
Notoginsenoside Ft1 (NGFt1), a dammarane triterpene glycoside isolated from Panax notoginseng, showed potent effective in stimulating platelet aggregation in our previous assay, yet its pharmacokinetic behavior is still unclear. This study describes a rapid and sensitive ultra-high-pressure LC–tandem mass spectrometry assay for determining of NGFt1 in rat plasma. Methanol-mediated precipitation was used for sample pre-treatment. Chromatographic separation was achieved on a C18 column with gradient elution using water and acetonitrile as mobile phase. Determination was obtained using an electrospray ionization source in negative selected reaction monitoring (SRM) mode at the transitions of m/z 915.9 → m/z 783.8 and m/z 799.8 → m/z 637.8 for NGFt1 and internal standard, respectively. The assay was linear over the concentration range 0.25–2500 ng/mL (r > 0.995) with the lower limit of quantification of 0.25 ng/mL. The intra- and inter-day precisions (relative standard deviation, %) ranged 1.65%–9.84% and 2.46%–13.49%, respectively, whereas accuracy (relative recovery, %) ranged from 96.21% to 99.45%, respectively. The recovery ranged from 95.09% to 102.22% and the matrix effect from 98.29% to 100.13%. The analyte was stable under tested storage conditions. The method has been successfully applied to a preclinical pharmacokinetic study in rats after a single intravenous (2 mg/kg) and oral (50 mg/kg) administration.
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