A capillary gas chromatographic method using flame ionization detection was developed and validated for the trace quantification of 2-bromoethanol (2-BE) and 2-bromoethylmethanesulfonate (2-BEM) in silodosin, used in the treatment of benign prostatic hyperplasia. Chromatographic separation was performed in spilt mode using nitrogen as carrier gas on a column containing crosslinked polyethylene glycol (30 m × 0.32 mm, 0.25 µm) stationary phase modified with nitroterephthalic acid. A simple matrix precipitation strategy was implemented to eliminate the sample overload and the matrix interference problems. The developed method was linear and accurate in the concentration range of 24–3000 ppm for 2-BE and 24–300 ppm for 2-BEM with r2 ˃ 0.999 and percent recoveries greater than 90% for both the analytes. The developed method was precise for both the analytes with RSD(%) of not more than 4.5%. In silico genotoxicity and carcinogenicity potential of 2-BEM were assessed using ICH M7 principles. The developed method can be applied in the quality control laboratories of pharmaceutical industries for trace level quantification of 2-BE and 2-BEM in silodosin.

中文翻译：

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使用毛细管气相色谱法对西洛多辛中的两种遗传毒性杂质进行计算机毒性评估和痕量定量

开发并验证了一种使用火焰离子化检测的毛细管气相色谱法，用于对用于治疗良性前列腺增生的西洛多辛中的 2-溴乙醇 (2-BE) 和 2-溴乙基甲磺酸盐 (2-BEM) 进行痕量定量。使用氮气作为载气在含有用硝基对苯二甲酸改性的交联聚乙二醇（30 m × 0.32 mm，0.25 µm）固定相的色谱柱上以溢出模式进行色谱分离。实施简单的基质沉淀策略以消除样品过载和基质干扰问题。所开发的方法在 2-BE 的 24–3000 ppm 和 2-BEM 的 24–300 ppm 浓度范围内呈线性且准确，两种分析物的 r2 ˃ 0.999 和回收率均大于 90%。所开发的方法对两种分析物均准确，RSD(%) 不超过 4.5%。使用 ICH M7 原则评估了 2-BEM 的计算机遗传毒性和致癌性潜力。所开发的方法可应用于制药行业的质量控制实验室，对赛洛多辛中的 2-BE 和 2-BEM 进行痕量定量。