基于绿色、多功能高通量微井氧化的分光光度法测定胶囊中加洛韦的含量。

Green and Versatile High-Throughput Microwell Oxidation-Based Spectrophotometric Methods for Determination of Galidesivir in Capsules.

机构信息

Department of Pharmaceutical Chemistry, College of Pharmacy, King Saud University, PO Box 2457, Riyadh 11451, Saudi Arabia.

出版信息

J AOAC Int. 2024 Oct 1;107(5):727-734. doi: 10.1093/jaoacint/qsae047.

DOI:10.1093/jaoacint/qsae047

PMID:38870529

Abstract

BACKGROUND

Galidesivir (GDV) is a promising new antiviral drug for the potent and safe treatment of a broad spectrum of viral diseases, including COVID-19. In the literature, no analytical method exists for the determination of GDV in bulk and dosage form.

OBJECTIVE

The aim of this study was the development of versatile green and simple microwell spectrophotometric methods (MW-SPMs) for the determination of GDV in its bulk form and capsules.

METHODS

Three MW-SPMs were developed involving the oxidation of GDV by ammonium metavanadate (AMV), chromium trioxide (CTO), and potassium iodate (PIO) in an acid medium. The reactions were carried out in 96-well plates at room temperature and the absorbances of chromogenic reaction products were measured by an absorbance microplate reader at 780, 595, and 475 nm for AMV, CTO, and PIO, respectively. Variables influencing the reactions were carefully investigated and optimized.

RESULTS

Linear relations with excellent correlation coefficients (0.9991-0.9997) were found between the absorbances and GDV concentrations in the range of 25-500 µg/mL. The LODs were ≥8.3 µg/mL. The accuracy and precision of the three MW-SPMs were confirmed by recovery and replicate analysis, respectively. The recovery values were 98.6-101.2% and the RSDs were ≤1.02%. The proposed MW-SPMs were successfully applied to the analysis of GDV in bulk drug and capsules with high accuracy and precision. The greenness of the MW-SPMs was confirmed by three comprehensive metric tools.

CONCLUSION

The proposed MW-SPMs combined the inherent advantages of microwell-based analysis and the use of common laboratory reagents for the reactions involved. These advantages include high-throughput, ready automation, reduced sample/reagent volume, precise measurements, and versatility. The advantages of the use of common laboratory reagents include availability, consistency, compatibility, safety, and cost-effectiveness.

HIGHLIGHTS

Overall, the proposed MW-SPMs are versatile valuable tools for the quantitation of GDV during its pharmaceutical manufacturing.

摘要

背景

加地昔韦（GDV）是一种很有前途的新型抗病毒药物，可有效且安全地治疗多种病毒疾病，包括 COVID-19。文献中尚无用于测定 GDV 原料药和制剂的分析方法。

目的

本研究旨在开发用于测定 GDV 原料药和胶囊制剂的多功能绿色、简便的微孔分光光度法（MW-SPM）。

方法

建立了三种 MW-SPM，分别涉及在酸性介质中用偏钒酸铵（AMV）、三氧化铬（CTO）和碘酸钾（PIO）氧化 GDV。反应在 96 孔板中于室温下进行，并用吸光度微板读数仪在 780、595 和 475nm 处分别测定显色反应产物的吸光度，以 AMV、CTO 和 PIO 分别对应。仔细研究并优化了影响反应的变量。

结果

在 25-500μg/mL 范围内，吸光度与 GDV 浓度之间呈现良好的线性关系，相关系数均≥0.9991-0.9997。检出限均≥8.3μg/mL。通过加标回收和重复性分析分别验证了三种 MW-SPM 的准确性和精密度。回收率为 98.6-101.2%，RSD≤1.02%。该 MW-SPM 成功应用于原料药和胶囊中 GDV 的分析，具有较高的准确度和精密度。通过三种综合度量工具证实了 MW-SPM 的绿色性。