Mahgoub Samar M, Alawam Abdullah S, Rudayni Hassan A, Allam Ahmed A, Ezzat Khaled Hesham, Elsuccary Saber A A, Radalla Abdelatty M, Mahmoud Rehab
Materials Science and Nanotechnology Department, Faculty of Postgraduate Studies for Advanced Sciences, Beni-Suef University, Egypt.
Department of Biology, College of Science, Imam Mohammad Ibn Saud Islamic University (IMSIU), Riyadh 11623, Saudi Arabia.
Anal Methods. 2025 Jul 31;17(30):6215-6230. doi: 10.1039/d5ay00698h.
Parkinson's disease (PD) remains a debilitating neurodegenerative disorder, with levodopa (LEV) as the cornerstone of its management. However, the long-term use of LEV is often complicated by motor fluctuations and dyskinesias, necessitating adjunct therapies such as carbidopa (CAR) and safinamide (SAF) to enhance efficacy and reduce side effects. Despite the promising therapeutic potential of this combination, the simultaneous analysis of the three drugs in pharmaceutical formulations poses significant analytical challenges. This study addresses this critical gap by developing and validating a sensitive and specific reversed-phase high-performance liquid chromatography (RP-HPLC) method for their simultaneous quantification in pure forms and in-house oral capsule formulations. The optimized method utilized a gradient elution using phosphate buffer (pH 3, 0.1 M) and acetonitrile as the mobile phase, a C8 stationary phase, and UV detection at 240 nm, achieving baseline separation within 11 min. Validation studies demonstrated excellent linearity, precision (RSD < 2%), accuracy (recovery 98.97-100%), and robustness, with LODs of 0.063 μg mL, 0.112 μg mL, and 0.058 μg mL, and LOQs of 0.190 μg mL, 0.341 μg mL, and 0.177 μg mL for LEV, CAR, and SAF, respectively. The in-house capsule formulation exhibited uniform drug content (90-110% of label claim), rapid disintegration (<8 min), and complete dissolution of LEV and CAR within 45 min, while SAF showed sustained release over 60 min. The method is offering a reliable and sustainable approach for quality control, pharmaceutical analysis, and industrial applications. The greenness profile of the method was rigorously evaluated using the NEMI, AGP, ESA, AGREE, and MoGAPI methods. Furthermore, the blueness of the technique was studied using the BAGI method, confirming its alignment with green analytical chemistry principles.
帕金森病（PD）仍然是一种使人衰弱的神经退行性疾病，左旋多巴（LEV）是其治疗的基石。然而，长期使用左旋多巴常常会出现运动波动和异动症等并发症，因此需要诸如卡比多巴（CAR）和沙芬酰胺（SAF）等辅助疗法来提高疗效并减少副作用。尽管这种联合用药具有可观的治疗潜力，但在药物制剂中同时分析这三种药物带来了重大的分析挑战。本研究通过开发并验证一种灵敏且特异的反相高效液相色谱（RP-HPLC）方法来解决这一关键差距，该方法可同时对其纯品形式以及自制口服胶囊制剂中的三种药物进行定量分析。优化后的方法采用以磷酸盐缓冲液（pH 3，0.1 M）和乙腈为流动相的梯度洗脱，C8固定相，并在240 nm处进行紫外检测，在11分钟内实现基线分离。验证研究表明该方法具有出色的线性、精密度（RSD < 2%）、准确度（回收率98.97 - 100%）和稳健性，左旋多巴、卡比多巴和沙芬酰胺的检测限分别为0.063 μg/mL、0.112 μg/mL和0.058 μg/mL，定量限分别为0.190 μg/mL、0.341 μg/mL和0.177 μg/mL。自制胶囊制剂显示出均匀的药物含量（为标签标示量的90 - 110%）、快速崩解（<8分钟），左旋多巴和卡比多巴在45分钟内完全溶解，而沙芬酰胺在60分钟内呈现缓释。该方法为质量控制、药物分析和工业应用提供了一种可靠且可持续的方法。使用NEMI、AGP、ESA、AGREE和MoGAPI方法对该方法的绿色度进行了严格评估。此外，使用BAGI方法研究了该技术的蓝色度，证实其符合绿色分析化学原则。
