Analytical reversed‐phase high‐performance liquid chromatography method development for silodosin and solifenacin in bulk and marketed formulation using analytical quality by design approach

The aim of this study was to develop and validate a robust reversed‐phase high‐performance liquid chromatography (RP‐HPLC) method for the simultaneous estimation of neomycin sulfate (NEO) and beclomethasone dipropionate (BECLO) in both bulk drug and pharmaceutical dosage forms. The analysis was conducted using the Box‐Behnken design. The separation of NEO and BECLO was conducted on a Phenomenex Luna C‐18 column (4.6 × 150 mm, 5 µm), employing a mobile phase comprising a mixture of methanol and trifluoroacetic acid in a ratio of 88:12% v/v. The separation was performed at a flow rate of 0.6 mL/min. NEO and BECLO were analyzed at a wavelength of 240 nm employing a photodiode array detector. The validation of the methodology followed the guidelines outlined in the International Council for Harmonization Q2 R (1). The validation process involved assessing critical parameters such as linearity, accuracy, system suitability, precision, and robustness. The results for each parameter were found to be within the acceptable range. The results indicate that the established RP‐HPLC method can effectively be employed for the routine analysis of NEO and BECLO in bulk drug and pharmaceutical dosage forms.

Section: Evaluation Of the Analytical Methods Employing The Qbd Approachmentioning

confidence: 99%

Quality by design‐engineered reversed‐phase high‐performance liquid chromatography method development and validation for simultaneous estimation of neomycin sulfate and beclomethasone dipropionate in bulk and pharmaceutical dosage form

Dessai,

Mannur,

Koli

et al. 2024

“…The Box-Behnken Design is a helpful technique for improving the outcomes in the field of chromatographic analysis [11,12]. Finding the most important factors that influenced the features of the liquid-liquid chromatographic separation, such as retention time, relative retention time, peak form and symmetry, tailing factor, and the number of theoretical plates, was one of the goals of this study [13][14][15]. A literature survey revealed that several methods are available for the determination of cefepime in different matrixes individually or in combination with other drugs like second-derivative spectroscopy [16], HPLC [17][18][19], and UPLC [20].…”

Section: Introductionmentioning

confidence: 99%

Reversed‐phase high‐performance liquid chromatography analytical method development and validation for cefepime and sulbactam injection formulation assay: A quality by design approach

Mondal

Asati

Verma

et al. 2023

A trustworthy high‐performance liquid chromatography approach for the simultaneous measurement of cefepime and sulbactam was created using quality by design. Finding reliable chromatographic settings for quality peaks and suitable component separation within a manageable run time was the key objective. Critical quality attributes for risk measurement were evaluated. To create an analytical design space and create a control strategy, the quantitative link between critical material attributes and critical quality attributes was built. Acetonitrile volume, trimethylamine volume, and flow rate were the three independent parameters considered in the mathematical models. Acetonitrile:high‐performance liquid chromatography water:triethylamine and pH 6.0, adjusted with orthophosphoric acid (50.0:50:0.15, v/v/v) as the mobile phase at 1.1 ml/min, were the ideal and anticipated conditions. We obtained appropriate baseline separation of both medications in about 10 min using these ideal conditions. The main determinant of the perturbation plot responses was found to be the quantity of acetonitrile. At all three levels, the percent recoveries for both medications ranged from 99% to 99.68%. Relative standard deviations were less than 2% for both drugs' intermediate accuracy and repeatability. A straightforward, precise, and repeatable high‐performance liquid chromatography method for regular quality control testing was created as a consequence.

“…A comprehensive literature search was conducted to find methods for the analysis of solifenacin succinate and silodosin alone or in combination with other medications. Most of these methods, which include ultraviolet (UV)visible spectrophotometry [10][11][12][13][14][15], spectrofluorometry [15], high-performance liquid chromatography (HPLC) [16][17][18][19][20][21][22][23][24][25][26][27][28], ultra-HPLC [29], liquid chromatography with electrospray ionization mass spectrometry [30], and high-performance thin layer chromatography (HPTLC) [31][32][33]. There is currently no greenness defined analytical method for measuring solifenacin succinate and silodosin in tablet dosage form together.…”

Section: Introductionmentioning

confidence: 99%

High‐performance thin layer chromatographic method development and validation for simultaneous estimation of solifenacin succinate and silodosin using quality by design approach and greenness assessment

Lodha,

Pillai,

Kalyankar

et al. 2023

The current research developed a high‐performance thin layer chromatographic method based on green analytical chemistry and integrated experimental approaches of analytical quality by design for simultaneous estimation of solifenacin succinate and silodosin. The integration was planned to reduce energy and solvent usage, maximize efficacy, and minimize any negative environmental effects. Taguchi design for screening and optimization a Box–Behnken design was used. The n‐butanol:ethanol:triethylamine (6:4:0.1, v/v/v) mobile phase and ultraviolet detection at 221 nm were used to develop the method. As per International Council for Harmonization Q2(R1) specifications, the method was validated. Rf value for solifenacin succinate and silodosin was found to be 0.29 ± 0.02 and 0.58 ± 0.02 respectively. For solifenacin succinate and silodosin, the linearity was found over the concentration ranges of 500–2500 ng/band and 800–4000 ng/band. For solifenacin succinate, the limits of detection and quantification were found to be 13.00 and 39.34 ng/band, respectively, while for silodosin, they were 33.29 and 100.86 ng/band, respectively. For solifenacin succinate, the method revealed a percent recovery ranging from 98.49% to 99.50%, while for silodosin, it exhibited a range from 98.86% to 99.79%. The tools predicted greenness score to be 63 and 0.78, respectively, indicating the proposed method to be green.