Background Chromatographic behavior of different substances in normal and reversed phases is an interesting area in the scientific community. Objective The work aimed to optimize and validate chromatographic separation methods for simultaneous determination of paracetamol (PAR) and phenylephrine HCl (PHE) in the presence of PAR impurities, namely p-aminophenol, p-nitrophenol, acetanilide, and p-chloroacetanilide with further quantification of these toxic impurities. Methods TLC method based on normal phase separation was carried out on aluminum sheets of silica gel 60 F254 using ethanol:chloroform:ammonia as a developing system, followed by densitometric measurements. While HPLC is based on reversed phase separation using a C18 column against acetonitrile:phosphate buffer pH 5 as a mobile phase. Results PAR and PHE were determined by the TLC-densitometric method in concentration ranges of 3–25 and 0.1–3 µg/band, respectively, and determined by the HPLC method over concentration ranges of 5–400 and 2–80 µg/mL, respectively. Both methods were optimized and validated. Furthermore, they were successfully applied for pharmaceutical formulations with precision <2%. Moreover, results of a statistical comparison with the official methods confirm the methods’ validity claims. Conclusion Two eco-friendly chromatographic methods were developed to determine PAR and PHE in their binary mixtures, pharmaceutical formulations, and in the presence of PAR-related impurities with further quantification of these toxic impurities. Highlights These simple chromatographic methods are the first methods developed for simultaneous determination of PAR and PHE in the presence of PAR-related impurities.

中文翻译：

---

对乙酰氨基酚杂质同时测定对乙酰氨基酚和盐酸去氧肾上腺素的正相和反相环保色谱方法的系统优化和验证

背景 不同物质在正相和反相中的色谱行为是科学界的一个有趣领域。目的 本工作旨在优化和验证色谱分离方法，以便在 PAR 杂质（即对氨基苯酚、对硝基苯酚、乙酰苯胺和对氯乙酰苯胺）存在下同时测定对乙酰氨基酚 (PAR) 和盐酸去氧肾上腺素 (PHE)，并进一步定量。这些有毒杂质。方法 以乙醇:氯仿:氨水为展开体系,对硅胶60 F254铝片进行正相分离薄层色谱法,进行光密度测定。而 HPLC 基于反相分离，使用 C18 色谱柱以乙腈：磷酸盐缓冲液 pH 5 作为流动相。结果 PAR 和 PHE 分别在 3-25 和 0.1-3 µg/波段的浓度范围内通过 TLC 光密度法测定，在 5-400 和 2-80 µg/mL 的浓度范围内通过 HPLC 法测定，分别。两种方法都经过优化和验证。此外，它们成功地应用于精确度<2%的药物制剂。此外，与官方方法的统计比较结果证实了该方法的有效性要求。结论 开发了两种环保色谱方法来测定二元混合物、药物制剂中的 PAR 和 PHE，并在存在 PAR 相关杂质的情况下进一步定量这些有毒杂质。