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用于测定醋氨己酸和吲哚美辛的环保色谱方法;绿色度评估。

Eco-Friendly Chromatographic Methods for Determination of Acemetacin and Indomethacin; Greenness Profile Assessment.

机构信息

Cairo University, Faculty of Pharmacy, Analytical Chemistry Department, Kasr El-Aini Street, ET-11562 Cairo, Egypt.

出版信息

J AOAC Int. 2021 Dec 11;104(6):1485-1491. doi: 10.1093/jaoacint/qsab085.

Abstract

BACKGROUND

The green chemistry approach was developed for the purpose of saving the environment by using green solvents. Applying green analytical chemistry principles to traditional methods is considered a challenge. Acemetacin is a commonly used analgesic prodrug that bioactivates to indomethacin.

OBJECTIVE

Developing two simple, eco-friendly chromatographic methods for simultaneous determination of acemetacin and indomethacin.

METHOD

The first method is HPLC-DAD. Separation was performed on a Waters XBridge® Shield RP18 (250 × 4.6 mm, 5 µm) analytical column with ethanol-ammonium acetate buffer (50 mM, pH 3.5 ± 0.1; 60:40, v/v) as a mobile phase at a flow rate of 1 mL/min at 25 ± 0.5°C and UV detection at 254 nm. The other method is TLC coupled with densitometric quantification using pre-coated silica TLC plates and butanol-ethyl acetate (70:30, v/v) elution system. The plates were scanned at 254 nm.

RESULTS

Both methods were validated according to International Conference on Harmonization guidelines. Linearity was confirmed for both over a concentration range of 1-100 µg/mL for the HPLC method and 0.2-7 µg/band for TLC-densitometric method. The methods' greenness was evaluated by the National Environmental Methods Index, Eco-Scale, Green Analytical Procedure Index metrics and Analytical GREEnness Metric Approach.

CONCLUSIONS

The proposed methods were found to be suitable for determination of studied drugs in their marketed formulations and is suggested for routine analysis in quality control laboratories.

HIGHLIGHTS

The developed HPLC method shortened the elution time of the analyzed drugs saving more time and money and the TLC method lowered the drugs' detection limit. HPLC and TLC methods were validated for the assay of acemetacin and indomethacin. The methods' greenness was evaluated and compared to published methods. The developed HPLC method shortened the elution time of the analyzed drugs, saving time and money and the TLC method lowered the drugs' detection limit.

摘要

背景

绿色化学方法的开发目的是通过使用绿色溶剂来保护环境。将绿色分析化学原则应用于传统方法被认为是一项挑战。醋氨芬是一种常用的镇痛前药,可生物转化为吲哚美辛。

目的

开发两种简单、环保的色谱方法,用于同时测定醋氨芬和吲哚美辛。

方法

第一种方法是 HPLC-DAD。分离在 Waters XBridge®Shield RP18(250×4.6mm,5μm)分析柱上进行,以乙醇-乙酸铵缓冲液(50mM,pH3.5±0.1;60:40,v/v)为流动相,流速为 1mL/min,在 25±0.5°C 下进行,在 254nm 处进行紫外检测。另一种方法是 TLC 与密度定量相结合,使用预涂覆的硅胶 TLC 板和正丁醇-乙酸乙酯(70:30,v/v)洗脱系统。将板在 254nm 处扫描。

结果

两种方法均根据国际协调会议指南进行验证。HPLC 方法的线性范围为 1-100μg/mL,TLC-密度法定量法的线性范围为 0.2-7μg/带。通过国家环境方法指数、生态标度、绿色分析程序指数和分析绿色度方法评估对方法的绿色度进行了评估。

结论

所提出的方法被发现适用于测定市售制剂中研究药物的含量,并建议在质量控制实验室中进行常规分析。

要点

所开发的 HPLC 方法缩短了分析药物的洗脱时间,节省了时间和金钱,TLC 方法降低了药物的检测限。HPLC 和 TLC 方法均用于测定醋氨芬和吲哚美辛。对方法的绿色度进行了评估,并与已发表的方法进行了比较。所开发的 HPLC 方法缩短了分析药物的洗脱时间,节省了时间和金钱,TLC 方法降低了药物的检测限。

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