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采用混合模式色谱柱和荷电气溶胶检测器开发并验证了一种用于测定托吡酯的稳定性指示 HPLC 方法。

Development and validation of a stability-indicating HPLC method for topiramate using a mixed-mode column and charged aerosol detector.

机构信息

Department of Pharmaceutics, Faculty of Pharmacy, Federal University of Rio de Janeiro, Rio de Janeiro, RJ, Brazil.

Department of Chemistry and Biochemistry, University of Texas at Arlington, Arlington, TX, USA.

出版信息

J Sep Sci. 2018 Apr;41(8):1716-1725. doi: 10.1002/jssc.201701340. Epub 2018 Feb 20.

Abstract

The analysis of topiramate in the presence of its main degradation products is challenging due to the absence of chromophore moieties and their wide range of polarity. Mixed-mode chromatography has been used in such cases because it combines two or more modes of separation. Charged aerosol detector is also an alternative since its detection is independent of optical properties and analyte ionization. This study is aimed to develop and validate two new stability-indicating methods by high-performance liquid chromatography for the main degradation products of topiramate using mixed-mode chromatography and a charged aerosol detector. Method 1 employed an Acclaim Trinity P1® column (3.0 mm × 150 mm, 2.7 μm) with a mobile phase comprising of 80% ammonium acetate buffer (20 mM, pH 4.0) and 20% methanol at a flow rate of 0.5 mL/min at 35°C. Method 2 utilized a C18 Acclaim 120® column (4.6 mm × 250 mm; 5 μm) with ACN/water (50:50) at a flow rate of 0.6 mL/min at 50°C. Validation of the two methods demonstrated excellent performance with respect to linearity, precision, accuracy, and selectivity. The limits of detection for topiramate, fructose, sulfate, sulfamate, and compound A were 2.97, 12.08, 4.02, 13.91, and 3.94 μg/mL, respectively.

摘要

由于缺乏生色团部分及其广泛的极性,在存在其主要降解产物的情况下分析托吡酯具有挑战性。在这种情况下,已经使用了混合模式色谱法,因为它结合了两种或更多种分离模式。由于其检测独立于光学性质和分析物的离子化,因此也可以使用带电气溶胶检测器。本研究旨在开发和验证两种新的稳定性指示方法,通过使用混合模式色谱法和带电气溶胶检测器的高效液相色谱法,对托吡酯的主要降解产物进行分析。方法 1 采用 Acclaim Trinity P1 ® 柱(3.0mm×150mm,2.7μm),流动相由 80%乙酸铵缓冲液(20mM,pH4.0)和 20%甲醇组成,流速为 0.5mL/min,在 35°C 下进行。方法 2 采用 C18 Acclaim 120 ® 柱(4.6mm×250mm;5μm),以 ACN/水(50:50)为流动相,流速为 0.6mL/min,在 50°C 下进行。对这两种方法的验证表明,它们在线性、精密度、准确度和选择性方面具有出色的性能。托吡酯、果糖、硫酸盐、磺胺酸盐和化合物 A 的检测限分别为 2.97、12.08、4.02、13.91 和 3.94μg/mL。

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