Ultrafast Liquid Chromatographic Method Development and its Validation for Quantification of Telaprevir in Pharmaceutical Dosage Form by Using Quality by Design Approach

Dutta

et al. 2021

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A new combination of metoprolol succinate, telmisartan, and cilnidipine is recently approved to treat hypertension effectively. A reversed‐phase liquid chromatography method was developed to quantify the said compounds, combining analytical eco‐scale and quality‐by‐design approach. The former one revealed an excellent green score for the present method. Later, method variables were assessed for risks and optimized using the quality‐by‐design‐oriented method development. The optimization process included using a Box‐Behnken design, and the obtained response surfaces for resolution amongst target peaks were mapped systematically. The optimal separation conditions employed a mobile phase of methanol: 0.01 M KH2PO4 buffer of pH 3.0 (70:30, %v/v) flowing at a rate of 1.0 mL/min on a C18 column with diode array detection at 240 nm. All three analyte peaks were well separated from each other with a resolution greater than 2.0. The analytical method was linear (2.5‐80 μg/mL) for target compounds with accuracy (>99%), and precision (<1%) results complying with regulatory requirements. The results of detection and quantitation limits, solution stability, and system suitability limit were good and acceptable. The current method selectively quantified the analytes from commercial dosage forms. Overall a green analytical method is developed and suitable for estimating metoprolol, telmisartan, and cilnidipine simultaneously in their combined pharmaceutical formulations.

Section: Quality By Design Workflowmentioning

confidence: 99%

Analytical eco‐scale and quality by design‐oriented liquid chromatography method for simultaneous quantification of metoprolol succinate, telmisartan, and cilnidipine in their fixed‐dose combination

Dutta

et al. 2021

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“…The ICH Q8 (R2) provides flexibility to pharmaceutical research and development community by allowing exploring the basic and vital steps of the QbD approach . This rapid QbD approach is not only time‐efficient and economic during the analytical development phase but also produces commensurate results those obtained by traditional extensive QbD workflow . It has only three but vital steps such as the establishment of analytical target profile (ATP) and critical analytical attributes (CAAs) considering the critical method variables (CMVs), selection of a befitting analytical technique and defining analytical control strategies (ACS).…”

Section: Introductionmentioning

confidence: 99%

“…This rapid QbD approach is not only timeefficient and economic during the analytical development Abbreviations: ACS, (Analytical control strategy); ATP, (Analytical target profile); CAAs, (Critical analytical attributes); CMVs, (Critical method variables); DPN, (Daptomycin); PDA, (Photodiode array); QbD, (Quality by design); UFLC, (Ultrafast liquid chromatography); YRT, (Youden's robustness test). phase but also produces commensurate results those obtained by traditional extensive QbD workflow [3][4][5][6]. It has only three but vital steps such as the establishment of analytical target profile (ATP) and critical analytical attributes (CAAs) considering the critical method variables (CMVs), selection of a befitting analytical technique and defining analytical control strategies (ACS).…”

Section: Introductionmentioning

confidence: 99%

Development and validation of a quality by design enabled robust LC method for estimation of daptomycin in pharmaceutical dosage form

Pradhan

2019

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A simple and new validated liquid chromatography method with stability‐indicating potential was established for quantifying daptomycin in formulations using a quality by design approach. Analytical target profile establishment and earmarking critical analytical attributes helped to control the method performance. Further, the control strategies for critical method variables were defined as per method intent. Youden's robustness test was applied with the dual intent of defining control strategies and evaluating method robustness for continuous method improvement. Chromatography for the purpose constituted of methanol: water (pH 3.5 maintained by o‐phosphoric acid), 90:10, v/v as mobile phase flowing at 1.2 mL/min on a C18 column. Photodiode array detector provided the best results at 367 nm. Results for parameters viz. linearity (5‐200 µg/mL), accuracy (> 99%) and precision (< 1%) advocated method reliability. The detection (2.5 µg/mL) and quantitation limits (5 µg/mL) were quite in agreement with method need. In a nutshell, the hyphenation of Youden's test with quality by design approach ensured the development of a reliable chromatography method for routine estimation of daptomycin throughout its product lifecycle.

“…The fishbone diagram effectively segregates various method variables, and the vital ones are further subjected to C‐N‐X approach . The variables are then systematically optimized using experimental designs for attaining desired performance . The identified CMVs are investigated using the design of experiments (DoE) to minimize the effect of variability on method performance and optimize the experimental conditions.…”

Section: Introductionmentioning

confidence: 99%

Analytical lifecycle management approach: Application to development of a reliable LC method for estimation of lacidipine

Acharjya

et al. 2019

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Lack of quality analytical methods with assured robustness and reliability has always been a serious concern for drug regulatory agencies. In the present study, a contemporary approach of analytical life‐cycle management resulted in the robust and reliable chromatographic analysis of lacidipine at a retention time of 5.1 min on a C‐18 column. Method variables such as %acetonitrile, flow rate, and pH were optimized using the design of experiment approach and their effect on critical quality attributes was studied. The attributes of the present study were significantly influenced by %acetonitrile and flow of the mobile phase. The newly optimized method was validated for various parameters with values in accordance with federal guidance. The lifecycle approach proved to be beneficial for routine application with a potential of future bio‐analytical utility.