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液相色谱-电喷雾电离质谱法对大鼠血浆中白术内酯III进行定量测定。

Quantitative determination of atractylenolide III in rat plasma by liquid chromatography electrospray ionization mass spectrometry.

作者信息

Wang Rui, Wang GuangJi, Hao Haiping, Xie HaiTang, Zhang Jinfeng, Wu Feng

机构信息

Key laboratory of Drug Metabolism and Pharmacokinetics, China Pharmaceutical University, 24 Tong Jia Xiang Street, Mail Box 210, Nanjing 210009, Jiangsu Province, China.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2006 Feb 2;831(1-2):36-41. doi: 10.1016/j.jchromb.2005.11.026. Epub 2005 Dec 1.

Abstract

Atractylenolide III is a major active component in Atractylodes macrocephala. This paper describes a simple, rapid, specific and sensitive method for the quantification of atractylenolide III in rat plasma using a liquid-liquid extraction procedure followed by liquid chromatography mass spectrometric (LC-MS) analysis. A Kromasil 3.5 microm C(18) column (150 mm x 2.00 mm) was used as the analytical column. Linear detection responses were obtained for atractylenolide III concentration ranging from 5 to 500 ng L(-1). The precision and accuracy data, based on intra-day and inter-day variations over 5 days were within 10.29%. The lower limit of quantitation for atractylenolide III was 5 ng mL(-1), using 0.1 mL plasma for extraction and its recoveries were greater than 85% at the low, medium and high concentrations. The method has been successfully applied to a pharmacokinetic study in rats after an oral administration of atractylenolide III with a dose of 20.0 mg kg(-1). With the lower limits of quantification at 5 ng mL(-1) for atractylenolide III, this method was proved to be sensitive enough for the pharmacokinetics study of atractylenolide III.

摘要

白术内酯III是白术中的主要活性成分。本文描述了一种简单、快速、特异且灵敏的方法,用于定量大鼠血浆中的白术内酯III。该方法采用液-液萃取步骤,随后进行液相色谱-质谱(LC-MS)分析。使用Kromasil 3.5微米C(18)柱(150毫米×2.00毫米)作为分析柱。白术内酯III浓度在5至500纳克/升范围内可获得线性检测响应。基于5天内的日内和日间变化,精密度和准确度数据在10.29%以内。白术内酯III的定量下限为5纳克/毫升,采用0.1毫升血浆进行萃取,其在低、中、高浓度下的回收率均大于85%。该方法已成功应用于大鼠口服20.0毫克/千克剂量白术内酯III后的药代动力学研究。由于白术内酯III的定量下限为5纳克/毫升,该方法被证明对白术内酯III的药代动力学研究足够灵敏。

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