Marzouk Hoda M, Ibrahim Engy A, Hegazy Maha A, Saad Samah S
Analytical Chemistry Department, Faculty of Pharmacy, Cairo University, Kasr Al-Aini Street, 11562, Cairo, Egypt.
Pharmaceutical Analytical Chemistry Department, College of Pharmaceutical Sciences and Drug Manufacturing, Misr University for Science & Technology, 6 of October City, Giza, Egypt.
Microchem J. 2022 Jul;178:107400. doi: 10.1016/j.microc.2022.107400. Epub 2022 Mar 19.
Nowadays, all researchers are focused on combating the pandemic COVID-19. According to recent statistics, most patients are managed at home. An over-the-counter (OTC) triple action formula containing paracetamol (PAR), aspirin (ASP), and diphenhydramine (DIPH) is widely prescribed for pain, fever and as night-time sleep aid. For COVID-19 patients, this combination is now suggested as part of symptomatic therapy and prophylaxis. In this work, two simple liquid chromatographic approaches were designed for simultaneous determination of PAR, ASP, and DIPH in Excedrin® PM caplets, beside three specified official toxic impurities, namely, -aminophenol, -nitrophenol, and salicylic acid. The first method comprised high-performance thin-layer chromatographic separation coupled with densitometric quantification, on silica gel HPTLC 60 F aluminium sheets as the stationary phase, ethyl acetate-methanol-aqueous ammonium hydroxide (10.0: 2.0: 0.1, by volume) as the developing system and scanning was performed at 210.0 nm. The second one is a high-performance liquid chromatography coupled with diode array detector. Successful separation of the six components was performed on XTerra C column with isocratic elution of mobile phase 0.1% triethylamine acidified water: methanol (70:30, v/v) adjusted with -phosphoric acid to pH 3.0 and methanol (90:10, v/v) with flow rate programming and detection at 210.0 nm. Validation of the proposed methods was performed according to ICH guidelines. Both methods were successfully used for quality control of the cited drugs in their marketed formulation. Moreover, the in-vitro release study was monitored using the proposed HPLC-DAD method. The greenness profile of the proposed methods was assessed and comparatively evaluated through various assessment tools, specifically; the analytical eco-scale system, national environmental method index (NEMI), green analytical procedure index (GAPI) and analytical greenness (AGREE) metric.
如今，所有研究人员都专注于抗击新冠疫情。根据最近的统计数据，大多数患者在家中接受治疗。一种含有对乙酰氨基酚（PAR）、阿司匹林（ASP）和苯海拉明（DIPH）的非处方（OTC）三联配方药物被广泛用于止痛、退烧以及作为夜间助眠药物。对于新冠患者，这种组合现在被建议作为对症治疗和预防的一部分。在这项工作中，设计了两种简单的液相色谱方法，用于同时测定艾德维尔PM胶囊中的PAR、ASP和DIPH，以及三种特定的法定有毒杂质，即对氨基酚、对硝基苯酚和水杨酸。第一种方法包括在硅胶HPTLC 60 F铝片作为固定相、乙酸乙酯 - 甲醇 - 氢氧化铵水溶液（体积比为10.0: 2.0: 0.1）作为展开系统的条件下，进行高效薄层色谱分离并结合密度定量法，扫描波长为210.0 nm。第二种方法是高效液相色谱结合二极管阵列检测器。在XTerra C柱上，以流动相0.1%三乙胺酸化水:甲醇（70:30，v/v）用磷酸调节至pH 3.0和甲醇（90:10，v/v）进行等度洗脱，并通过流速程序控制，在210.0 nm波长处进行检测，成功分离了这六种成分。所提出的方法按照国际人用药品注册技术协调会（ICH）指南进行了验证。这两种方法都成功用于所提及药物上市制剂的质量控制。此外，使用所提出的HPLC - DAD方法监测了体外释放研究。通过各种评估工具，特别是分析生态规模系统、国家环境方法指数（NEMI）、绿色分析程序指数（GAPI）和分析绿色度（AGREE）指标，对所提出方法的绿色度概况进行了评估和比较。
