胶束液相色谱在绿色化学中的应用：抗血小板固定剂量复方制剂质量控制分析中的应用。

Micelle-Incorporated Liquid Chromatography in the Light of Green Chemistry: An Application for the Quality Control Analysis of Anti-Platelet Fixed-Dose Combinations.

机构信息

Egyptian Russian University, Faculty of Pharmacy, Department of Analytical Chemistry, Cairo, Egypt.

Zagazig University, Faculty of Pharmacy, Department of Analytical Chemistry, Zagazig, Egypt.

出版信息

J AOAC Int. 2022 Sep 6;105(5):1228-1233. doi: 10.1093/jaoacint/qsac046.

DOI:10.1093/jaoacint/qsac046

PMID:35595172

Abstract

BACKGROUND

Oral anti-platelet agents are the cornerstone of the treatment of multiple cardiovascular diseases and in the long-term prevention of their recurrence.

OBJECTIVE

In the present work, we report a method based on micellar liquid chromatography coupled with ultraviolet detection (MLC/UV), for the simultaneous quantification of combined anti-platelet therapy namely, clopidogrel bisulfate (CPS), aspirin (ASP), together with salicylic acid (SA), in their pharmaceutical dosage form.

METHODS

The incorporation of 0.1M polyoxyethylene 23 lauryl ether (Brij-35) as a surfactant into the mobile phase improved solute-mobile phase interaction allowing for minimal organic solvent utilization, enhanced resolution, and rapid analysis (7 min). Furthermore, we performed a comprehensive evaluation of the environmental impact caused by our procedures versus previously reported analytical procedures applied in the determination of CPS and ASP. The evaluation was made using the Eco-scale tool.

RESULTS

The results of the developed method indicated the superiority of our procedures in terms of greenness without compromising the quality of performance characteristics. The method was linear in the range of 1-100 µg/mL with limits of detection of 0.28, 0.32, and 0.29 µg/mL for CPS, ASP, and SA, respectively. The developed method can also be utilized to test the purity and the stability of ASP in pharmaceutical formulations through monitoring SA as its main degradation product.

CONCLUSION

The MLC/UV method was successfully applied to the quantitative analysis of CPS, ASP together with SA-as a main degradation product of ASP-in their pharmaceutical dosage form.

HIGHLIGHTS

The developed method was successfully applied for the determination of clopidogrel bisulfate (CPS), aspirin (ASP), together with salicylic acid (SA), in their pharmaceutical dosage form.

摘要

背景

口服抗血小板药物是治疗多种心血管疾病和预防其复发的基石。

目的

本工作报道了一种基于胶束液相色谱法结合紫外检测（MLC/UV）的方法，用于同时定量分析联合抗血小板治疗药物，即硫酸氢氯吡格雷（CPS）、阿司匹林（ASP）和水杨酸（SA）在其药物制剂中的含量。

方法

在流动相中加入 0.1M 聚氧乙烯 23 月桂醚（Brij-35）作为表面活性剂，改善了溶质-流动相相互作用，减少了有机溶剂的使用，提高了分辨率，并实现了快速分析（7 分钟）。此外，我们对我们的方法相对于之前报道的用于测定 CPS 和 ASP 的分析方法在环境影响方面进行了全面评估。使用生态尺度工具进行了评估。

结果

所开发方法的结果表明，我们的方法在不影响性能特征质量的情况下在绿色性方面具有优越性。该方法在 1-100μg/mL 范围内呈线性，CPS、ASP 和 SA 的检测限分别为 0.28、0.32 和 0.29μg/mL。该方法还可用于通过监测 SA 作为其主要降解产物来测试 ASP 药物制剂的纯度和稳定性。