A Quality-Driven, Eco-friendly High-Performance Thin-Layer Chromatography Method for Fluvoxamine Maleate Analysis in Tablets and MS Identification of its Degradation Products

IF 1.3 4区化学 Q4 BIOCHEMICAL RESEARCH METHODS

Chromatographia Pub Date : 2025-06-19 DOI:10.1007/s10337-025-04417-4

Vidhya K. Bhusari, Prasad S. Giri, Minal R. Ghante

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Abstract

Introduction

A common selective serotonin reuptake inhibitor used to treat depression and obsessive–compulsive disorder is fluvoxamine maleate.

Objective

The goal of this study was to develop and validate a HPTLC method for the analysis of fluvoxamine maleate in pharmaceutical dosage forms, utilizing a risk-based quality by design approach.

Methods

HPTLC method was optimized with a mobile phase composed of toluene: ethyl acetate: methanol: triethylamine in a ratio of 1: 5: 4: 0.1 (v/v/v/v). UV detection was performed at 257 nm. Studies on forced degradation were carried out in a variety of stress environments, including as thermal, oxidative, hydrolytic, alkaline, acidic, and photolytic conditions, to assess stability of fluvoxamine maleate. The degradation products were characterized using high-resolution mass spectrometry to identify potential impurities and degradation pathways.

Results

The developed method demonstrated excellent linearity over a concentration range of 100 to 600 ng/band, with a correlation coefficient of 0.9994 and the LOD and LOQ values were found to be 15.36 ng/band and 46.55 ng/band. The method was validated in accordance with ICH Q2(R1) guidelines, confirming its specificity, linearity, precision, accuracy, and robustness. The green chemistry aspects of the method were evaluated using Analytical Greenness Metric Approach and Software and Green Analytical Procedure Index, which highlighted the method’s eco-friendly characteristics. Additionally, the Blue Applicability Grade Index tool was used to assess the method’s practicality and suitability for routine pharmaceutical analysis, confirming its application in real-world settings.

Conclusion

The validated HPTLC method for analyzing fluvoxamine maleate in tablet dosage forms was robust, reliable, and accurate. It effectively identified and characterized degradation products, ensuring the consistent quality and safety of pharmaceutical products. The method offers a sustainable and efficient alternative for quality control in the pharmaceutical industry, combining rigorous validation with environmentally conscious practices.

Graphical Abstract

Abstract Image

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质量驱动、生态友好型马来酸氟伏沙明片的高效薄层色谱分析及其降解产物的质谱鉴定

常用的选择性血清素再摄取抑制剂是马来酸氟伏沙明，用于治疗抑郁症和强迫症。目的利用基于风险的质量设计方法，建立并验证一种高效液相色谱（HPTLC）分析马来酸氟伏沙明的方法。方法以甲苯：乙酸乙酯：甲醇：三乙胺为流动相，流动相比为1:5:4:0.1 (v/v/v/v)，对色谱法进行优化。在257 nm处进行紫外检测。为了评估马来酸氟伏沙明的稳定性，在热、氧化、水解、碱性、酸性和光解等多种应激环境下进行了强制降解研究。利用高分辨率质谱法对降解产物进行表征，以确定潜在的杂质和降解途径。结果该方法在100 ~ 600 ng/波段范围内线性良好，相关系数为0.9994，检出限和定量限分别为15.36 ng/波段和46.55 ng/波段。根据ICH Q2（R1）指南对该方法进行验证，确认其特异性、线性度、精密度、准确度和鲁棒性。使用分析绿色度量方法和软件以及绿色分析程序指数对该方法的绿色化学方面进行了评估，这突出了该方法的环保特性。此外，使用蓝色适用性等级指数工具评估该方法在常规药物分析中的实用性和适用性，确认其在实际环境中的应用。结论建立的高效液相色谱法分析马来酸氟伏沙明片剂的方法可靠、准确。它有效地识别和表征了降解产物，确保了药品的一致质量和安全。该方法结合了严格的验证和环保意识实践，为制药行业的质量控制提供了一种可持续和有效的替代方法。图形抽象

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来源期刊

Chromatographia 化学-分析化学

CiteScore

3.40

自引率

5.90%

发文量

103

审稿时长

2.2 months

期刊介绍： Separation sciences, in all their various forms such as chromatography, field-flow fractionation, and electrophoresis, provide some of the most powerful techniques in analytical chemistry and are applied within a number of important application areas, including archaeology, biotechnology, clinical, environmental, food, medical, petroleum, pharmaceutical, polymer and biopolymer research. Beyond serving analytical purposes, separation techniques are also used for preparative and process-scale applications. The scope and power of separation sciences is significantly extended by combination with spectroscopic detection methods (e.g., laser-based approaches, nuclear-magnetic resonance, Raman, chemiluminescence) and particularly, mass spectrometry, to create hyphenated techniques. In addition to exciting new developments in chromatography, such as ultra high-pressure systems, multidimensional separations, and high-temperature approaches, there have also been great advances in hybrid methods combining chromatography and electro-based separations, especially on the micro- and nanoscale. Integrated biological procedures (e.g., enzymatic, immunological, receptor-based assays) can also be part of the overall analytical process.