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采用液相色谱-串联质谱法测定大鼠血浆中的竹节香附甲素:在药代动力学研究中的应用。

Determination of Raddeanin A in rat plasma by liquid chromatography-tandem mass spectrometry: application to a pharmacokinetic study.

机构信息

Department of Pharmacology, Institute of Medical Sciences, Shanghai Jiao Tong University School of Medicine, Shanghai 200025, China.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2013 Apr 1;923-924:43-7. doi: 10.1016/j.jchromb.2013.01.019. Epub 2013 Feb 4.

Abstract

A simple, rapid and sensitive LC-MS/MS analysis method was developed and validated for the determination of Raddeanin A (RA) in rat plasma. Protein precipitation with three volumes of methanol as the precipitation reagent was used as the sample preparation method. The analysis process was performed on a Thermo Syncronis C18 column with the mobile phase of methanol-water (containing 5mM ammonium formate, pH 2.2) (85:15, v/v). RA and glycyrrhetinic acid (internal standard) were monitored under negative electrospray ionization in multiple reaction monitoring (MRM) mode. Retention time of RA and IS were 2.1 min and 3.5 min, respectively. The limit of detection was 5 ng/mL and the linear range was 50-50,000 ng/mL. The intra-day and inter-day precision was 1.87-2.94% and 3.25-5.36%, and the intra-day and inter-day accuracy ranged from 5.9% to 10.5% and 5.6% to 11.1%, respectively. The absolute recovery was above 90.3%. The method has been successfully translated to the pharmacokinetic study of RA in rats after intravenous and intraperitoneal administration (0.75 mg/kg).

摘要

建立并验证了一种用于测定大鼠血浆中栀子苷 A(RA)的简单、快速和灵敏的 LC-MS/MS 分析方法。采用甲醇三倍沉淀法作为样品前处理方法,以甲醇-水(含 5mM 甲酸铵,pH2.2)(85:15,v/v)为流动相,在 Thermo Syncronis C18 柱上进行分析。RA 和甘草次酸(内标)在负离子电喷雾电离多反应监测(MRM)模式下进行监测。RA 和 IS 的保留时间分别为 2.1 min 和 3.5 min。检测限为 5 ng/mL,线性范围为 50-50,000 ng/mL。日内和日间精密度分别为 1.87-2.94%和 3.25-5.36%,日内和日间准确度分别为 5.9%-10.5%和 5.6%-11.1%。绝对回收率均高于 90.3%。该方法已成功应用于 RA 静脉注射和腹腔注射(0.75 mg/kg)后在大鼠体内的药代动力学研究。

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