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高效液相色谱法和圆二色光谱法测定胶囊中纳多洛尔的四种立体异构体

Determination of Four Nadolol Stereoisomers in Capsules by High-Performance Liquid Chromatography and Circular Dichroism.

作者信息

Prado Alexandre Grazielle, Wandermuren Márcio Nardelli, Peron Adriano, Tavares Vanessa Franco, Ramalho Padeiro Denis Alexandre, Sakiara Kelly Alessandra, Aurora-Prado María Segunda, Singh Anil Kumar, Kedor-Hackmann Erika Rosa, Miritello Santoro Maria Inês Rocha

机构信息

University of São Paulo, Faculty of Pharmaceutical Sciences, Department of Pharmacy, Avenida Professor Lineu Prestes 580, CEP 05508-000 São Paulo, SP, Brazil.

出版信息

J AOAC Int. 2017 Jul 1;100(4):1016-1022. doi: 10.5740/jaoacint.16-0292. Epub 2017 Jan 21.

DOI:10.5740/jaoacint.16-0292
PMID:28109074
Abstract

Nadolol is a blocking agent with activity in β-adrenergic receptors. The objective of this research was to develop and validate an HPLC and circular dichroism method for the quantification of four nadolol stereoisomers in capsules. The HPLC method was validated using a Chiralcel OD column (250 × 4,6 mm, 10 μm). The mobile phase consisted of hexane-ethanol-diethylamine-acetic acid (86 + 14 + 0.3 + 0.3, v/v/v/v), with a flow rate of 0.7 mL/min and temperature of 25 ± 1°C and UV detection carried out at 220 nm. Solutions were prepared in ethanol containing 200 μg/mL nadolol. The method proved to be precise, selective, accurate, and robust and was successfully applied for the determination of the two homologs of four nadolol stereoisomers in capsules.

摘要

纳多洛尔是一种对β-肾上腺素能受体有活性的阻滞剂。本研究的目的是开发并验证一种用于定量胶囊中四种纳多洛尔立体异构体的高效液相色谱法和圆二色性方法。高效液相色谱法使用Chiralcel OD柱(250×4.6 mm,10μm)进行验证。流动相由己烷 - 乙醇 - 二乙胺 - 乙酸(86 + 14 + 0.3 + 0.3,v/v/v/v)组成,流速为0.7 mL/min,温度为25±1°C,在220 nm处进行紫外检测。溶液在含有200μg/mL纳多洛尔的乙醇中制备。该方法被证明是精确、选择性好、准确且稳健的,并成功应用于测定胶囊中四种纳多洛尔立体异构体的两种同系物。

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