El-Masry Amal A, Zeid Abdallah M, Abdallah Nora A
Department of Medicinal Chemistry, Faculty of Pharmacy, Mansoura University, Mansoura, 35516, Egypt.
Department of Chemistry, Michigan University, AnnArbor, MI, 48103, USA.
BMC Chem. 2025 May 5;19(1):117. doi: 10.1186/s13065-025-01477-3.
The Food and Drug Administration recently approved a fixed dose combination of aspirin and omeprazole that has been introduced for the treatment of gastrointestinal disorders, as it reduces the risk of upper gastrointestinal and cardiovascular adverse events in aspirin-treated patients. Therefore, an optimized eco-friendly, simple, fast, and precise quantitative nuclear magnetic resonance spectroscopy technique was presented for the concurrent estimation of that mixture in their single and combined dosage forms. The quantitative nuclear magnetic resonance spectroscopy concurrent estimation of both drugs was achieved using phloroglucinol as the internal standard and dimethyl sulfoxide as a deuterated solvent. An ideal set of acquisition parameters was determined to be 128 scans, 10 s relaxation latency, and 90° pulse angle. The selected quantitative signal of aspirin was the doublet of doublet signal appeared at 7.945 ppm, while that of omeprazole was the singlet signal at 8.18 ppm. The singlet signal at 5.69 ppm was selected for the internal standard. The spectra were subjected to integration, baseline correction, and auto phase correction. The developed quantitative proton nuclear magnetic resonance spectroscopy method was found to be rectilinear over the range of 0.05-4.0 mg mL for both drugs. The detecting and quantifying limits for both drugs were approximately 0.01 and 0.03 mg mL, respectively. Neither labelling nor pretreatment steps were needed to assay the studied drugs using our developed quantitative nuclear magnetic resonance spectroscopy method. The proposed nuclear magnetic resonance spectroscopy approach was effectively evaluated in terms of linearity (r = 0.9999), accuracy, and precision (%RSD < 1.08). Furthermore, the suggested technique was investigated to analyze the studied drugs in their single and combined dosages. This work enables clinicians to simultaneously monitor aspirin and omeprazole levels in both single and fixed-dose combination tablets, ensuring precise dosing and effective treatment management. For patients, it supports safer therapy by reducing the risks associated with improper dosing or drug interactions in combination therapies. After evaluating the method's greenness, whiteness and blueness, it was determined that the suggested approach was environmentally friendly. The suggested approach was compared with the previously reported methods from both an analytical and eco-friendly perspective.
美国食品药品监督管理局最近批准了一种阿司匹林和奥美拉唑的固定剂量复方制剂，该制剂已被用于治疗胃肠道疾病，因为它可降低接受阿司匹林治疗患者发生上消化道和心血管不良事件的风险。因此，本文提出了一种优化的、环保、简单、快速且精确的定量核磁共振光谱技术，用于同时测定该混合物的单一剂型和复方剂型。以间苯三酚为内标，二甲亚砜为氘代溶剂，实现了两种药物的定量核磁共振光谱同时测定。确定的理想采集参数为128次扫描、10秒弛豫延迟和90°脉冲角。阿司匹林选定的定量信号是出现在7.945 ppm处的双二重峰信号，而奥美拉唑的定量信号是8.18 ppm处的单峰信号。内标选择5.69 ppm处的单峰信号。对光谱进行积分、基线校正和自动相位校正。所建立的定量质子核磁共振光谱法在两种药物0.05 - 4.0 mg/mL范围内呈线性关系。两种药物的检测限和定量限分别约为0.01和0.03 mg/mL。使用我们开发的定量核磁共振光谱法测定所研究的药物，无需标记或预处理步骤。所提出的核磁共振光谱方法在线性度（r = 0.9999）、准确度和精密度（%RSD < 1.08）方面得到了有效评估。此外，还对所建议的技术进行了研究，以分析所研究药物的单一剂型和复方剂型。这项工作使临床医生能够同时监测单一片剂和固定剂量复方片剂中阿司匹林和奥美拉唑的水平，确保精确给药和有效的治疗管理。对于患者而言，它通过降低联合治疗中不当给药或药物相互作用相关的风险，支持更安全的治疗。在评估该方法的绿色度（绿度、白度和蓝度）后，确定所建议的方法是环境友好的。从分析和环境友好的角度将所建议方法与先前报道的方法进行了比较。
