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在联用法(紫外和带电气溶胶检测)杂质分析中,流动相组成对维加特林的影响。

Influence of the mobile phase composition on hyphenated ultraviolet and charged aerosol detection for the impurity profiling of vigabatrin.

机构信息

University of Würzburg, Institute for Pharmacy and Food Chemistry, 97074, Würzburg, Germany.

University of Würzburg, Institute for Pharmacy and Food Chemistry, 97074, Würzburg, Germany.

出版信息

J Pharm Biomed Anal. 2021 Jul 15;201:114110. doi: 10.1016/j.jpba.2021.114110. Epub 2021 May 3.

Abstract

Recently, charged aerosol detection (CAD), a universal detection technique in liquid chromatography, has been introduced into monographs of the European Pharmacopoeia (Ph. Eur.), which now employs HPLC-UV-CAD for assessing the impurities of the drug vigabatrin. The separation of vigabatrin and its impurities is facilitated by ion pair chromatography (IPC) in the compendial method using tridecafluoroheptanoic acid (TDFHA) as ion-pairing reagent. However, the subsequent detection of the impurities by UV-CAD is considerably impaired due to the substantial amount of ion-pairing reagent applied in the method generating high levels of background noise. In this study, the influence of the mobile phase composition on the background noise of the CAD was evaluated applying response surface methodology. The model's results indicated that the chain length of the ion-pairing reagent is a predominant factor for noise generation. Thus, an alternative method for the impurity analysis of vigabatrin using mixed-mode chromatography (MMC) instead of IPC was developed. The dual separation mechanism of the MMC column enabled the choice of a mobile phase better suited for the individual requirements of the UV-CAD detectors, while maintaining excellent selectivity. The MMC method does not require the addition of a post-column solution to reduce the TDFHA concentration in the mobile phase, and, therefore, needs less instrumentation. Moreover, the sample concentration could be halved due to the improved LOQs of the impurities (<50 ng on column) and the analysis time could be shortened (30 to 20 min) due to improved separation efficiency. The MMC method was validated with respect to ICH guideline Q2(R1).

摘要

最近,荷电气溶胶检测(CAD)作为一种通用的液相色谱检测技术,已被引入欧洲药典(Ph. Eur.)专论中,该专论现在采用 HPLC-UV-CAD 来评估药物氨己烯酸的杂质。在药典方法中,采用十三氟庚酸(TDFHA)作为离子对试剂,通过离子对色谱(IPC)分离氨己烯酸及其杂质。然而,由于该方法中应用了大量的离子对试剂,会产生高水平的背景噪声,因此后续通过 UV-CAD 检测杂质的效果会受到很大影响。在本研究中,应用响应面法评估了流动相组成对 CAD 背景噪声的影响。模型结果表明,离子对试剂的链长是产生噪声的主要因素。因此,开发了一种使用混合模式色谱(MMC)代替 IPC 分析氨己烯酸杂质的替代方法。MMC 柱的双重分离机制使我们能够选择更适合 UV-CAD 检测器个别要求的流动相,同时保持出色的选择性。MMC 方法不需要添加柱后溶液来降低流动相中 TDFHA 的浓度,因此需要的仪器较少。此外,由于杂质的 LOQs(<50ng 柱上)提高,样品浓度可以减半,由于分离效率提高,分析时间可以缩短(30 分钟至 20 分钟)。该 MMC 方法已根据 ICH 指南 Q2(R1)进行了验证。

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