Darweish Eman, Marzouk Hoda M, Fayez Yasmin M, Eissa Maya S
Department of Pharmaceutical Chemistry, Faculty of Pharmacy, Egyptian Russian University, Badr City, Egypt.
Department of Analytical Chemistry, Faculty of Pharmacy, Cairo University, Cairo, Egypt.
J Sep Sci. 2023 Jan;46(1):e2200695. doi: 10.1002/jssc.202200695. Epub 2022 Nov 3.
Nowadays, Green Analytical Chemistry is widely applied to provide various analytical methods with eco-friendly procedures employing the least toxic, harmful reagents on humans and the environment without affecting the efficacy of the determination. Accordingly, two eco-friendly, accurate, and reliable high-performance thin-layer chromatography-densitometry and high-performance liquid chromatographic methods were established for the determination and separation of two antispasmodic drugs, namely phloroglucinol and trimethylphloroglucinol in their pure, combined dosage form along with phloroglucinol toxic impurity, 3,5-dichloroaniline. For high-performance thin-layer chromatography-densitometry, efficient separation was developed via utilizing the stationary phase of high-performance thin-layer chromatography silica gel 60 F plates and developing a system comprising of ethyl acetate-butanol-ammonia in the ratio of 8.0:2.0:0.2, by volume and scanning of the developed bands at 210.0 nm. The subsequent method is isocratic high-performance liquid chromatography with diode array detection in which separation was successively attained using XTerra RP-C (250 × 4.6 mm, 5 μm) column as stationary phase and methanol-10.0 mM phosphate buffer, pH 3.7 ± 0.1 as mobile phase in the ratio of 75.0:25.0, v/v at flow rate 1.0 ml/min and scanning at 220.0 nm. The developed liquid chromatography methods were validated according to the International Council for Harmonization guidelines, and all results acknowledged their efficacy. Additionally, the proposed methods worked well for assessing the cited drugs in binary combined commercially available pharmaceutical formulation. The greenness profile of the present methods was assessed and estimated using various assessment tools, namely; Green Analytical Procedure Index, analytical eco-scale method, National Environmental Method Index in addition to Analytical GREEnness tool to evaluate the greenness of the provided methods with a statistical comparison between them to assess the more green ones.
如今，绿色分析化学被广泛应用，以提供各种分析方法，这些方法采用对人类和环境毒性最小、危害最小的试剂，且环保程序不影响测定的有效性。因此，建立了两种环保、准确且可靠的高效薄层色谱 - 密度测定法和高效液相色谱法，用于测定和分离两种解痉药物，即间苯三酚和三甲基间苯三酚，它们以纯品、复方剂型存在，同时还含有间苯三酚有毒杂质3,5 - 二氯苯胺。对于高效薄层色谱 - 密度测定法，通过使用高效薄层色谱硅胶60 F板作为固定相，并开发一种体积比为8.0:2.0:0.2的乙酸乙酯 - 丁醇 - 氨组成的展开系统，在210.0 nm处扫描展开的谱带，实现了有效分离。后续方法是采用二极管阵列检测的等度高效液相色谱法，其中使用XTerra RP - C（250×4.6 mm，5μm）柱作为固定相，甲醇 - 10.0 mM磷酸盐缓冲液（pH 3.7±0.1）作为流动相，体积比为75.0:25.0，流速为1.0 ml/min，并在220.0 nm处扫描，依次实现分离。所开发的液相色谱方法根据国际协调理事会指南进行了验证，所有结果均证实了其有效性。此外，所提出的方法在评估二元复方市售药物制剂中的上述药物时效果良好。使用各种评估工具，即绿色分析程序指数、分析生态规模法、国家环境方法指数以及分析绿色度工具，对本方法的绿色度进行了评估和估计，并对它们进行统计比较以评估更绿色的方法。
