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Quantification and Validation of Stability-Indicating RP-HPLC Method for Efavirenz in Bulk and Tablet Dosage Form using Quality by Design (QbD): A Shifting Paradigm
Journal of Chromatographic Science ( IF 1.5 ) Pub Date : 2021-05-03 , DOI: 10.1093/chromsci/bmab061
Vishal C Gurumukhi 1 , Sanjaykumar B Bari 2
Affiliation  

The present study endeavors quality by design (QbD) assisted chromatographic method for the quantification of Efavirenz (ERZ) in bulk and tablet dosage form. Analytical QbD instigated with assignment of analytical target profile (ATP) and critical analytical attributes (CAAs). Risk assessment studies and factor screening studies facilitate to identify the critical method parameters (CMPs). Optimization was performed by employing 32 full factorial design using identified CMPs i.e., flow rate (X1) and pH of buffer (X2) at three different levels and evaluating selected CAAs i.e., retention time (Y1) and peak area (Y2). The individual and interactive influence of CMPs on CAAs were tested by statistical data and response surface plots. Analysis of variance (ANOVA) confirmed that method parameters are significant (P < 0.05). Chromatographic separation was achieved using methanol, 10 mM ammonium acetate buffer (70:30 v/v), pH adjusted at 3.1 with 0.05% ortho-phosphoric acid as a mobile phase at flow rate 1.0 mL/min, and a Nucleosil C18 (4.6 mm I.D. × 250 mm, 5 μm) column with UV detection at 247 nm. The method validation and subsequent stresses degradation studies according to ICH guidelines supported the method to be highly efficient for regular drug analysis and its degradation products. The proposed method was successfully demonstrated QbD based approach for the development of highly sensitive, reliable and suitable for routine analysis, and clinical applications.

中文翻译:

使用质量源于设计 (QbD) 的散装和片剂形式依非韦伦的稳定性指示 RP-HPLC 方法的量化和验证:一个转变的范式

本研究致力于质量源于设计 (QbD) 辅助色谱法,用于定量散装和片剂剂型中的依法韦仑 (ERZ)。分析 QbD 通过分配分析目标配置文件 (ATP) 和关键分析属性 (CAA) 发起。风险评估研究和因素筛选研究有助于确定关键方法参数 (CMP)。通过采用 32 种全因子设计进行优化,使用已确定的 CMP,即流速 (X1) 和缓冲液的 pH 值 (X2) 在三个不同的水平,并评估选定的 CAA,即保留时间 (Y1) 和峰面积 (Y2)。通过统计数据和响应面图测试了 CMP 对 CAA 的个体和交互影响。方差分析 (ANOVA) 证实方法参数是显着的 (P < 0.05)。使用甲醇、10 mM 乙酸铵缓冲液 (70:30 v/v) 实现色谱分离,使用 0.05% 正磷酸作为流动相以 1.0 mL/min 的流速将 pH 调节至 3.1,以及 Nucleosil C18 (4.6 mm ID × 250 mm, 5 μm) 色谱柱,紫外检测波长为 247 nm。根据 ICH 指南进行的方法验证和随后的应力降解研究支持该方法对常规药物分析及其降解产物非常有效。所提出的方法成功地证明了基于 QbD 的方法,用于开发高度敏感、可靠且适用于常规分析和临床应用的方法。× 250 mm, 5 μm) 色谱柱,紫外检测波长为 247 nm。根据 ICH 指南进行的方法验证和随后的应力降解研究支持该方法对常规药物分析及其降解产物非常有效。所提出的方法成功地证明了基于 QbD 的方法,用于开发高度敏感、可靠且适用于常规分析和临床应用的方法。× 250 mm, 5 μm) 色谱柱,紫外检测波长为 247 nm。根据 ICH 指南进行的方法验证和随后的应力降解研究支持该方法对常规药物分析及其降解产物非常有效。所提出的方法成功地证明了基于 QbD 的方法,用于开发高度敏感、可靠且适用于常规分析和临床应用的方法。
更新日期:2021-05-03
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