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采用 Box-Behnken 设计开发、评估关键方法变量并评估稳定性,以测定中枢作用肌肉松弛药物氯唑沙宗的药物制剂中的有机杂质。

Development, evaluation of critical method variables and stability assessment using a Box-Behnken design for the determination of organic impurities in a pharmaceutical dosage form of a centrally acting muscle relaxant drug chlorzoxazone.

机构信息

Department of Chemistry, School of Applied Sciences and Humanities (SASH), VIGNAN'S Foundation for Science, Technology & Research (VFSTR), Vadlamudi, India.

Laurus Generics, Inc., Berkeley Heights, New Jersey, USA.

出版信息

Biomed Chromatogr. 2024 Nov;38(11):e6001. doi: 10.1002/bmc.6001. Epub 2024 Sep 4.

Abstract

This study validates a stability-indicating LC method for detecting organic impurities in the chlorzoxazone dosage form. Using a Waters X-Select R HSS T3 analytical column, mobile phase of it was made by mixing of water, methanol, and glacial acetic acid in the ratio of 700:300:10 (v/v/v). The drug product and drug substance were subjected to the stress conditions such as acid, base, oxidation, heat, and photolysis as per the recommendations of the International Conference on Harmonization (Q2) methodology. The study revealed the susceptibility of 4-chloro-2-aminophenol to alkaline environments, emphasizing peak homogeneity and stability. The method verification, per ICH guidelines and USP<1225>, established precision, specificity, linearity, accuracy, and robustness for quality control. The mean impurity recovery ranged from 95.5% to 105.2%, the correlation coefficient (r) was greater than 1.000, and the RSD values (n = 6) ranged from 0.6% to 5.1% across the LOQ-150% ranges. Full-factorial design tested final method conditions, evaluating multiple parameters concurrently. Graphical optimization within the design space defined strong method requirements, ensuring consistent and reliable outcomes. The study develops and validates chlorzoxazone stability-indicating methods, employing advanced statistical approaches like design of experiments and factorial design, with resilient conditions established through graphical optimization of the design space.

摘要

本研究验证了一种可用于检测氯唑沙宗制剂中有关物质的稳定型 LC 方法。采用 Waters X-Select R HSS T3 分析柱,以水、甲醇和冰醋酸(700:300:10,v/v/v)的混合溶液作为流动相。按照国际协调会议(ICH)推荐的 Q2 方法,对药物产品和药物原料进行酸、碱、氧化、热和光解等条件的稳定性考察。研究结果表明,4-氯-2-氨基酚对碱性环境较为敏感,强调了峰的均一性和稳定性。根据 ICH 指南和 USP<1225>,对方法进行了验证,以确保精密度、专属性、线性、准确度和耐用性符合质量控制要求。杂质回收率的平均值在 95.5%至 105.2%之间,相关系数(r)大于 1.000,在 LOQ-150%范围内,RSD 值(n=6)的范围为 0.6%至 5.1%。全因子设计测试了最终方法条件,同时评估了多个参数。设计空间内的图形优化对方法提出了严格的要求,确保了结果的一致性和可靠性。本研究采用实验设计和全因子设计等先进的统计方法,开发并验证了氯唑沙宗的稳定性指示方法,通过设计空间的图形优化建立了有弹性的条件。

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