The present study aimed to develop a simple, robust, sensitive and effective stability-indicating reversed-phase high-performance liquid chromatography method for simultaneous quantification of diacerein (DCN) and aceclofenac (ACE) in novel nanoemulgel formulation and commercial tablets in the presence of their main degradation product: rhein (RH) and diclofenac sodium (DLS), respectively. A fractional factorial design was used to screen the crucial independent factors, whereas a central composite design was used for the optimization of the chromatographic conditions. The separation was carried out on Phenomenex C18 column (5 μm, 250 × 4.6 mm), using a mobile phase consisting of phosphate buffer pH 3 (0.1% v/v orthophosphoric acid) and acetonitrile (40:60 v/v) at a flow rate of 1 mL/min with detection at 264 nm. The analytes were exposed to a variety of stress conditions, including heat, alkali, acid, oxidation, photochemical, humidity and hydrolysis. DCN, ACE, RH and DLS were found to have retention times of 4.32 ± 0.15, 5.77 ± 0.07, 8.28 ± 0.20 and 9.10 ± 0.18 min, respectively. The percent recovery for all four analytes was found to be between 98 and 102, and the procedure was discovered to be linear in the range of 0.1–64 μg/mL with R2 value > 0.999. The established method was validated as per ICH guidelines and successfully used to assay DCN and ACE in their combined marketed tablet dosage form and developed nanoemulgel formulation.

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An innovative RP-HPLC technique was devised to simultaneously quantify thymoquinone (TQ) and capecitabine (CAP) in newly designed polymeric nanoparticles. A unique chromatographic approach was created, optimized and validated using Design-Expert® (design of experiment) in compliance with ICH requirements. A 24 factorial design examined the influence of variables on method responses. The method found linear between 0.25 and 16 μg/mL, with an R2 value of 0.999. The detection and quantification limits for CAP were 0.05 and 0.16 μg/mL, respectively, and 0.12 and 0.38 μg/mL for TQ, respectively, and 97–100% recovery in plain drug solution and 100–102% in nanoformulation were achieved. A purposeful modification examined by analysis of variance revealed that the experimental model was significant (P = 0.0001). The total drug content in nanoformulation was 8.68 mg, and the entrapment efficiency was 84.79%. Based on the findings, it is possible to infer that the use of the Quality by Design methodology resulted in the development of a more accurate technique capable of producing consistent, dependable, high-quality data and precise in quantifying CAP and TQ in bulk and nanoparticulate systems.

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Background: Fisetin (FIS) is a bioactive flavonoid found in various plants, reported for many pharmacological activities, and presently marketed as a nutraceutical. To overcome less water solubility and bioavailability issues, FIS cubosomal nanoformulation has been prepared and characterized. Objective: To estimate FIS in prepared novel cubosomes, an RP-HPLC analytical method development with the most sensitivity, economical, robust, and wide applicability in marketed FIS formulations and plant extracts also. Method: An RP-HPLC method was developed and validated as per ICH Q2R1 guidelines by using C-18 Phenomenex Luna 5µ, 100A0 column, LC-20 AD pump, and Shimadzu LC solution 1.25 software. The combination of acetonitrile and formic acid (0.1%v/v) in the ratio of 25:75 v/v was used as a mobile phase for chromatographic separation using a PDA detector at 360 nm and a flow rate of 1 ml/min. Results: In the range of 0.1 to 16 µg/ml, the developed method was remarkably linear (R2 ˃ 0.999). This method was found to be accurate (recovery 98.24 to 100.65 %), precise, robust (% RSD ˂ 2), and more sensitive than the earlier reported method with LOD and LOQ values of 17.26 and 52.31 ng/ml respectively. The FIS estimation was also performed using the developed method in the marketed FIS formulation Doctor’s Best ® Fisetin, and different plants extracts such as strawberry, grapes, black tea, and green tea. The forced degradation study suggests FIS was unstable in alkaline and oxidative stress conditions. Conclusion: For FIS estimation in cubosomal nanoformulation, a widely applicable, novel, robust, most sensitive, and economical RP-HPLC method was developed and validated, and also applied to marketed formulation and plant extracts.