Magdy Maimana A, Abdelrahman Maha M, Mohamed Doaa G, Ahmed Amal B
Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Beni-Suef University, Alshaheed Shehata Ahmad Hegazy St, Beni-Suef, 62514, Egypt.
Pharmaceutical Chemistry Department, Faculty of Pharmacy, Nahda University, Sharq El-Nile, Beni-Suef, 62511, Egypt.
BMC Chem. 2025 Jan 28;19(1):26. doi: 10.1186/s13065-025-01385-6.
The study of green analytical chemistry has garnered significant attention in the context of mitigating global environmental contamination. In this study, we present two methodologies for environmentally friendly chromatography that enable simultaneous and specific determination of Saxagliptin (SAX), metformin (MET), and a pharmacopoeial impurity of MET known as melamine (MEL). The initial method employed in this study is High-Performance Thin Layer Chromatography (HPTLC), which utilized 60 F 254 silica gel-coated Mark HPTLC plates on aluminum sheets as the stationary phase. The developing system was made up of a mix of ethyl acetate: methanol: ammonia: glacial acetic acid in a ratio of 6:4:1:0.3 (v/v/v/v). The analysis was performed at a wavelength of 215 nm. The second method employed in this study is ultra-performance liquid chromatography (UPLC). In this method, a C18 column was utilized for the separation process. The mobile phase was made up of a mix of methanol and 0.01 M sodium dodecyl sulfate, with a pH of 3.3 achieved by adding orthophosphoric acid. The ratio of methanol to sodium dodecyl sulfate in the mobile phase was 70:30 (v/v). The flow rate of the mobile phase was established at a rate of 1.5 mL/min. The peaks found and recorded are resolved at a wavelength of 215 nm. The three analytes under investigation were successfully separated and assessed using the recommended protocols. Both methods were validated following the International Council for Harmonization (ICH) recommendations for assessing linearity, range, accuracy, precision, specificity, and robustness. Moreover, the environmental sustainability of the advanced methodologies The assessment has been performed using various instruments, such as the Analytical Eco-Scale, NEMI, GAPI, and AGREE. The utilization of these tools was implemented in order to perform a comprehensive assessment of the environmental sustainability of the methods, as well as to establish a comparison with previously documented approaches. This study was carried out to evaluate the potential environmental implications of the suggested methods and to determine their suitability for concurrent analysis of the examined pharmaceuticals in formula and quality control units.
在减轻全球环境污染的背景下，绿色分析化学的研究已引起广泛关注。在本研究中，我们提出了两种环境友好型色谱分析方法，可同时特异性测定沙格列汀（SAX）、二甲双胍（MET）以及MET的一种药典杂质三聚氰胺（MEL）。本研究采用的第一种方法是高效薄层色谱法（HPTLC），它使用铝板上涂覆有60 F 254硅胶的Mark HPTLC板作为固定相。展开系统由乙酸乙酯：甲醇：氨水：冰醋酸按6:4:1:0.3（v/v/v/v）比例混合而成。分析在215 nm波长下进行。本研究采用的第二种方法是超高效液相色谱法（UPLC）。在此方法中，使用C18柱进行分离过程。流动相由甲醇和0.01 M十二烷基硫酸钠混合而成，通过添加正磷酸使pH值达到3.3。流动相中甲醇与十二烷基硫酸钠的比例为70:30（v/v）。流动相流速设定为1.5 mL/min。检测到并记录的峰在215 nm波长处得到分离。使用推荐方案成功分离并评估了所研究的三种分析物。两种方法均按照国际协调理事会（ICH）关于评估线性、范围、准确度、精密度、特异性和稳健性的建议进行了验证。此外，还使用各种工具（如分析生态量表、NEMI、GAPI和AGREE）对先进方法的环境可持续性进行了评估。使用这些工具是为了全面评估方法的环境可持续性，并与先前记录的方法进行比较。开展本研究是为了评估所建议方法可能对环境产生的影响，并确定它们在配方和质量控制单元中对所检测药物进行同时分析的适用性。
