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一种用于大鼠血浆中杜鹃素定量分析的灵敏超高效液相色谱-串联质谱法的建立与验证:在药代动力学和生物利用度研究中的应用

Development and validation of a sensitive UHPLC-MS/MS method for quantitative analysis of farrerol in rat plasma: Application to pharmacokinetic and bioavailability studies.

作者信息

Piao Li, Zang Mingcui, Gu Yue, Liu Baohua

机构信息

Department of Gynecology, the First Hospital of Jilin University, Changchun, Jilin, 130021, China.

Department of Hepatopancreatobiliary Surgery, the First Hospital of Jilin University, Changchun, Jilin, 130021, China.

出版信息

Biomed Chromatogr. 2017 Nov;31(11). doi: 10.1002/bmc.4005. Epub 2017 May 30.

Abstract

Farrerol is a 2,3-dihydro-flavonoid isolated from rhododendron. In this study, a sensitive and selective ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method was developed for the determination of farrerol in rat plasma. Liquid-liquid extraction by ethyl ether was used for sample preparation. Chromatographic separation was achieved on an Agilent UHPLC XDB-C column (2.1 × 100 mm, 1.8 μm) with water and methanol (30:70, v/v) as the mobile phase. An electrospray source was applied and operated in negative ion mode; selection reaction monitoring was used for quantification using target fragment ions m/z 299 → 179 for farrerol and m/z 267 → 252 for internal standard. Calibration plots were linear in the range of 2.88-1440 ng/mL for farrerol in rat plasma. Intra- and inter-day precisions were <11.6%, and the accuracy ranged from -13.9 to 11.9%. The UHPLC-MS/MS method was successfully applied in pharmacokinetics and bioavailability studies of farrerol in rats.

摘要

杜鹃素是从杜鹃花中分离得到的一种2,3-二氢黄酮类化合物。在本研究中,建立了一种灵敏且选择性高的超高效液相色谱-串联质谱(UHPLC-MS/MS)法,用于测定大鼠血浆中的杜鹃素。采用乙醚液-液萃取法进行样品制备。在Agilent UHPLC XDB-C柱(2.1×100 mm,1.8μm)上,以水和甲醇(30:70,v/v)作为流动相进行色谱分离。采用电喷雾源,在负离子模式下运行;选择反应监测用于定量分析,杜鹃素的目标碎片离子为m/z 299→179,内标的目标碎片离子为m/z 267→252。大鼠血浆中杜鹃素的校准曲线在2.88-1440 ng/mL范围内呈线性。日内和日间精密度均<11.6%,准确度范围为-13.9%至11.9%。该UHPLC-MS/MS方法成功应用于大鼠体内杜鹃素的药代动力学和生物利用度研究。

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