Liquid chromatography interfaced with mass spectroscopy (LC–MS) is a sensitive and effective analytical method that combines high-resolution separation as well as specific mass detection of impurities in formulated products and as well as in active pharmaceutical ingredient (API). In this study, LC–MS/MS was used to determine impurities formed during the stability period of Efinaconazole (EFZ, a triazole antifungal agent). The method was validated for its assay parameters such as specificity, linearity, accuracy, precision and also for solution stability. The calibration curve was found to be linear for the concentration range from 0.5 μg/mL to 30 μg/mL. A thorough investigation was performed by exposing Efinaconazole (1 mg/mL) to various stress conditions such as hydrolysis (acid and alkaline), oxidation, photolysis and temperature at various time intervals to achieve 10% degradation. The impurities formed during forced degradation were separated using high-performance liquid chromatography later it was identified using LC–MS/MS technique. The obtained results showed that EFZ is prone to oxidation when exposed to a 3% aqueous medium of hydrogen peroxide solution and quite stable in all the remaining stress conditions for a longer period.

中文翻译：

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LC-MS/MS 方法的开发和验证，用于分析抗真菌剂艾芬康唑应激研究过程中形成的杂质

液相色谱与质谱联用 (LC-MS) 是一种灵敏而有效的分析方法，它结合了高分辨率分离以及对制剂产品和活性药物成分 (API) 中杂质的特定质量检测。在本研究中，LC-MS/MS 用于确定艾芬康唑（EFZ，一种三唑类抗真菌剂）稳定期间形成的杂质。该方法的检测参数如特异性、线性、准确度、精密度以及溶液稳定性都得到了验证。发现校准曲线在 0.5 μg/mL 至 30 μg/mL 的浓度范围内呈线性。通过将艾芬康唑 (1 mg/mL) 暴露于各种压力条件，如水解（酸和碱）、氧化、光解和温度在不同的时间间隔达到10%的降解。使用高效液相色谱分离强制降解过程中形成的杂质，然后使用 LC-MS/MS 技术对其进行鉴定。所得结果表明，EFZ在暴露于3%过氧化氢溶液的水性介质中时容易氧化，并且在所有剩余应力条件下相当稳定较长时间。