Development and Validation of New Stability Indicating Reversed-Phase High-Performance Liquid Chromatography Method for Simultaneous Determination of Metformin Hydrochloride and Ertugliflozin in Bulk and Pharmaceutical Dosage Form

Objective: We have developed a “stability-indicating RP-HPLC” procedure for the Bilastine (BLS) and montelukast (MTL) analysis of tablets. Methods: The quantification of BLS and MTL combination was implemented utilising a Waters column (C18, 5 μm, 250 mm and 4.6 mm). Isocratic mobile phase had 60% volume KH2PO4 of 0.1M strength with pH 4.2 units and 40% volume methanol at a flow with 1.0 ml/min speed. UV detection at 232 nm was done to examine BLS and MTL. Stability experiments of BLS and MTL under distinctive environments of stress were also performed. Results: The BLS and MTL were eluted at 1.810 min and 2.551 min, respectively. The responses were found to be linear for the concentration ranges of 10-30 µg/ml (BLS) and 5-15 µg/ml (MTL). Percent comparative standard deviance for precision was 0.331% (BLS) and 0.486% (MTL). Percent assay for accuracy was 98.96% (BLS) and 99.00% (MTL). The detection limit and quantitation limit measures for BLS were 0.018 µg/ml and 0.059 µg/ml, respectively, while for MTL it was 0.024 µg/ml and 0.081 µg/ml, respectively. Robustness studies authorized that the method is robust with percent comparative standard deviance of a highest 1.950%. Conclusion: The developed “stability-indicating RP-HPLC” procedure for the BLS and MTL analysis is simple, sensitive, precise, specific and robust, making it appropriate to the assessment of BLS and MTL in a tablet formulation.

Section: Discussionmentioning

confidence: 99%

Quantification of Bilastine and Montelukast Combination in Formulations Utilizing Liquid Chromatography: Stability Studies

Vijayalakshmi¹,

Andrews

Rao³

2021

“…The standard and sample solutions were stable at room temperature and in refrigerator condition for two days in the selected diluent. It proved the ruggedness of the method [31]. LF degradation was more in the peroxide stress condition than that in the hydrolytic stress condition.…”

Section: Photolytic Degradationmentioning

confidence: 90%

“…The standard and sample solutions were kept at room temperature and at 2-8 °C for up to 48 h. These solutions were analyzed at 24 h and 48 h intervals and calculated the % difference from the initial area [31]. No major variations were found and verified that the solutions were stable up to 48 h. There is no effect in storage conditions for lumefantrine and its related impurities.…”

Section: Robustnessmentioning

confidence: 99%

The Development and Validation of a Fast Stability Indicating Rp-HPLC Method for Quantification of Lumefantrine and Its Organic Impurities Using Central Composite Experimental Design

RAMESH G.,

PRASAD

2023

Objective: The objective of the present study was to develop and validate a stability indicating RP-HPLC method for Lumefantrine (LF) and its organic impurities using a central composite design (CCD). Methods: A specific, simple quality control friendly isocratic elution method using reverse phase HPLC was developed for quantification of Lumefantrine (LF) and its organic impurities at a wavelength of 265 nm. The chromatographic separation was achieved on the column of Thermo Hypersil ODS C18 (150x4.6 mm, 3µ) with a buffer containing 0.1percent formic acid and acetonitrile 10:90 v/v as a mobile phase with a flow rate of 1.6 ml/min at 35 °C with a run time of 10 min. Based on the preliminary trials, CCD was employed to check the effect of independent variables such as Acetonitrile ratio (A), Flow rate (B), and Column oven temperature (C). While resolution between Lumefantrine (LF) and Impurity-A (X1), Impurity-A and Impurity-B (X2), and Plate count of Lumefantrine (LF) (X3) were considered as dependent variables and statistical evaluation performed by using design expert software. The optimized conditions were validated as per ICH guidelines. Results: The retention time of LF and its organic impurities were 1.9 min, 3.0, 4.5, and 6.4 min, respectively. Design space was established and desirability was found. LOD and LOQ for the Lumefantrine (LF) and its impurities were established with respect to test concentration. The plotted calibration curves were linear with a regression coefficient of R2>0.99, indicating that the linearity was within the limit. As a part of method validation, the parameters like Specificity with forced degradation, Linearity, Precision, Accuracy, Ruggedness, and Robustness were determined and the results were found to be within the allowable limits. Conclusion: The method developed and validated was found to be suitable for routine analysis and to be used for the measurement of Lumefantrine and its impurities. Since there is no stability indicating the RP-HPLC method with design space was reported in the literature, there is a need to develop quantitative methods under different conditions to achieve improvement in specificity and selectivity.

“…The specificity/selectivity of the chromatographic methodology was examined to confirm that there's no intervention from inactive ingredients of formulations, mobile phase solvents or/and stress degradants [30][31][32]. Interference from excipients, mobile phase at RT of AZIL and CILN has not been noticed, which proves selectivity for AZIL and CILN analysis in Myotan CN sample.…”

Section: Azil and Ciln Degradation Profilementioning

confidence: 98%

Quality Control Assay of Two Antihypertensive Representatives Using Rp-HPLC Based Methodology: Stress Assessment on Antihypertensive Representatives

KUMAR

Mandal

2022

Objective: A quick simultaneous separation and quality control assay of two antihypertensive representatives, Azilsartan (AZIL) and Cilnidipine (CLIN) in bulk and tablet formulation was developed and validated using a Reverse phase (RP) HPLC method within a run time of 10 min. Methods: All chromatographic separations of AZIL and CILN were operated on a “Supelco C18 column (250 × 4.6 mm, 5 μ)”, using a mobile phase of Na2SO4 (0.1 M, pH 4.0): methanol at 60:40 (v: v) ratio and the samples were analyzed at 239 nm. Stability assessments of AZIL and CILN were carried out as per the ICH Q1A (R2) regulation. The methodology for determining AZIL and CILN in bulk and formulations tablets was verified by adhering to International Conference on Harmonization (ICH) recommendations. Results: Retention times of AZIL and CILN samples were 4.023 and 5.732 min, respectively, indicating a quick elution time. Over the tested range of 20–60 µg/ml for AZIL and 5–15 µg/ml for CILN determination, calibration curves have displayed linearity and satisfactory results. LOD of AZIL and CILN are 0.083 µg/ml and 0.056 µg/ml, respectively. The approach suggested herein has satisfactory precision (RSD: 0.1013% for AZIL and 0.4944% for CILN) and accuracy (recovery: 99.20 to 100.34 % for AZIL and 100.17 to 101.59 % for CILN). Furthermore, the approach has also been shown to be effective in detecting degradants of AZIL and CILN and resolving them with high resolution. Conclusion: This approach is shown to be acceptable for the accurate quality control assay of two antihypertensive representatives, AZIL and CLIN in both bulk and tablet formulation.