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多种绿色光谱法用于测定厄多司坦原料药及其制剂的含量,并进行了广泛的绿色度评估。

Multiple green spectroscopic methods for erdosteine determination in bulk and dosage form with extensive greenness evaluation.

机构信息

Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy, Alexandria University, 1 El Khartoum Square, Alexandria, 21521, Egypt.

出版信息

Sci Rep. 2023 Oct 25;13(1):18216. doi: 10.1038/s41598-023-45334-6.

Abstract

Four simple, sensitive, economical, and eco-friendly spectrophotometric and spectrofluorimetric methods for the assay of erdosteine (ERD) in bulk and dosage form have been developed and validated as per the current ICH guidelines. Method I involved the addition of the powerful oxidizing agent, potassium permanganate to ERD and measuring the oxidation product at 600 nm. Another oxidizing agent; ceric ammonium sulfate was used in Method II where ERD is oxidized resulting in a decline in the absorbance intensity of cerium (IV) ions, measured at 320 nm. Similarly, Method III employed the use of ceric ammonium sulfate, However, the fluorescence intensity of the resulting cerium (III) ions was recorded at λex/λem 255/355 nm, respectively. Whereas in Method IV, ERD was added to acriflavine leading to a proportional decrease in its native fluorescence. Various reaction conditions affecting the intensity of measurement were attentively investigated, optimized, and validated. All the suggested methods did not require any tedious extraction procedures nor organic solvents. The implementation of the proposed methods in ERD assay resulted in linear relationships between the measured signals and the corresponding concentrations of ERD in the range of 1-6, 0.1-1.0, 0.01-0.1, and 10-100 μg/mL with LOD values 0.179, 0.024, 0.0027 and, 3.2 μg/mL for methods I, II, III and IV respectively. The suggested methods were successfully applied to ERD analysis in pure form and in commercial capsules. Furthermore, the eco-friendliness of the proposed methods was thoroughly checked using various greenness testing tools. Lastly, this work, not only presents highly sensitive, green, mix-and-read methods for ERD determination, but also, describes the determination of ERD spectrofluorimetrically for the first time in the literature.

摘要

四种简单、灵敏、经济且环保的分光光度法和荧光光度法已被开发并按照现行 ICH 指南进行验证,可用于测定厄多司坦(ERD)的含量。方法 I 涉及向 ERD 中加入强氧化剂高锰酸钾,并在 600nm 处测量氧化产物。另一种氧化剂——硫酸铈铵在方法 II 中被使用,其中 ERD 被氧化,导致铈(IV)离子的吸光度强度下降,在 320nm 处测量。同样,方法 III 也使用硫酸铈铵,但记录的是生成的铈(III)离子的荧光强度,激发波长/发射波长分别为 255/355nm。而在方法 IV 中,向吖啶黄素中加入 ERD,导致其本征荧光强度呈比例下降。仔细研究了影响测量强度的各种反应条件,并进行了优化和验证。所有建议的方法都不需要繁琐的提取程序或有机溶剂。在 ERD 测定中实施这些方法,导致测量信号与 ERD 的相应浓度之间呈线性关系,在 1-6、0.1-1.0、0.01-0.1 和 10-100μg/mL 的范围内,LOD 值分别为 0.179、0.024、0.0027 和 3.2μg/mL,用于方法 I、II、III 和 IV。这些方法已成功应用于 ERD 的纯品和商品胶囊分析。此外,还使用各种绿色测试工具彻底检查了所建议方法的环保性。最后,这项工作不仅提出了高度灵敏、绿色、混合读取的 ERD 测定方法,而且首次在文献中描述了 ERD 的荧光光度法测定。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8ed5/10600230/427dbd9fac0a/41598_2023_45334_Fig1_HTML.jpg

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