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Abstract Background Extensive literature review revealed that no RP–LC method has been developed for simultaneous estimation of EMPA, LINA and MET in combined dosage form. This is a newer combination approved by USFDA on 4th June 2019 and it is launch in the United State Market on 27th January 2020. Result A simple, sensitive, specific, precise and accurate reverse phase—high performance liquid chromatography (RP- HPLC) method has been developed for simultaneous estimation of Empagliflozin, Linagliptin and Metformin HCl in bulk and synthetic mixture. Phenomenex C18 column (250 mm × 4.6 mm, 5 µm) was used as stationary phase for chromatographic separation through isocratic elution using Acetonitrile: Methanol: Water in a ratio (27: 20: 53, v/v/v) pH 4 adjusted with 1% Ortho-phosphoric acid as mobile phase at flow rate 1 ml/min. PDA detector was used for simultaneous analysis of all three drugs at common wavelength 223 nm and the each injection volume was 20 µl. The linearity range for Empagliflozin, Linagliptin and Metformin HCl was found to be 0.5–5 µg/ml, 0.25–2.5 µg/ml, and 50–500 µg/ml, respectively. The retention time for Empagliflozin, Linagliptin and Metformin HCl was found to be 14.5 min, 3.4 min and 2.01 min, respectively. The percentage (%) recovery was found to be 99.98–100.81% for Empagliflozin, 99.33–100.57% for Linagliptin and 100.65–101.35% for Metformin HCl respectively. Conclusion As per the international Conference on Harmonisation (ICH) Q2 (R1) guideline, proposed RP–LC method validation has been carried out. The proposed RP–LC method was repeatable and selective as per statistical analysis and it can be use for simultaneous estimation of Empagliflozin, Linagliptin and Metformin HCl in bulk and synthetic mixture. The proposed method might be applied for simultaneous estimation of all three drugs in pharmaceutical formulation.

Abstract Background A sensitive, precise, and stability-indicating high-performance thin-layer chromatographic (HPTLC) method has been developed for the analysis of Remogliflozin etabonate in tablet formulation. HPTLC plates precoated with silica gel 60 F254 were used as the stationary phase; methanol: ethyl acetate: toluene: NH3 (2:4:4:0.1, v/v/v) was used as mobile phase, and densitometry was used for the quantitative estimation of the drug. The proposed method was validated with respect to linearity, accuracy, precision, and robustness and applied for the estimation of drug in tablet dosage form. Results The R f value of Remogliflozin etabonate was observed to be 0.61. The densitometric estimation was performed in reflectance mode at 229 nm. The method was found to be linear in the range of 500–8000 ng/band for Remogliflozin etabonate. The possible degradation pathway was estimated by performing forced degradation studies. The degradant peaks were well resolved from the drug peak with acceptable resolution in their R f value. Conclusion An accurate and precise high-performance thin-layer chromatographic method has been developed for the quantification of Remogliflozin etabonate in tablets. Forced degradation studies were performed, and drug was found to be highly susceptible to acid, base hydrolysis, and oxidative stress degradation and gets converted into active drug Remogliflozin. Both Remogliflozin etabonate and Remogliflozin bands were well resolved. The method was applied for the analysis of drug in tablet formulation, and it can be used for routine quality control analysis, as well as for the analysis of stability samples.

A precise and accurate method for the analysis of antihypertensive drug combination nifedipine and valsartan was developed using the HPTLC method. The stationary phase used was a pre-coated silica gel G60 – F254 aluminium sheet and the mobile phase was acetonitrile: methanol: n-butanol: acetic acid (6:2:2:0.1, v/v/v/v). The detection of spots was carried out densitometrically using a UV detector at 230 nm in the absorbance mode. The Rf values of valsartan and nifedipine were found to be 0.25 and 0.65, respectively. The calibration curve was found to be linear in the range of 120–320 ng/band and 900–2400 ng/band for nifedipine and valsartan, respectively. Forced degradation studies were performed using stress conditions like acid and base hydrolysis, photolytic, thermal and oxidative stress degradation to develop the stability indicating method. The degradation study indicated that nifedipine was susceptible to acid-base hydrolysis, oxidative stress degradation and photolytic degradation, while valsartan was susceptible to acid-base hydrolysis and oxidative stress degradation.

A sensitive, selective and precise high-performance thin-layer chromatographic method was developed and validated for the simultaneous determination of alprazolam and mebeverine, both as bulk drugs and in formulations. The method employed HPTLC aluminium plates that had been pre-coated with silica gel 60F-254 as the stationary phase, while the solvent system was acetone:methanol:acetic acid (6:4:0.1, v/v/v). The Rf values of alprazolam and mebeverine were observed to be 0.80 ± 0.08 and 0.60 ± 0.05, respectively. The densitometric analysis was carried out in absorbance mode at 225 nm. The linear regression analysis for the calibration plots showed a good linear relationship for alprazolam and mebeverine over concentration ranges of 600 to 3600 ng/spot and 1000 to 6000 ng/spot, respectively. The limit of detection and the limit of quantification for alprazolam (mebeverine) were determined to be 63.97 (11.35) ng/spot and 193.85 (34.40) ng/spot, respectively. Alprazolam and mebeverine stock solutions were subjected to acid and alkali hydrolysis, chemical oxidation, dry heat degradation and photo-degradation. Both drugs were found to be susceptible to acid and alkali hydrolysis, chemical oxidation and photo-degradation, whereas both were found to be stable towards dry heat. The degraded product peaks were well resolved from the pure drug peak and displayed a significant difference in their Rf values. Stressed samples were assayed using the developed HPTLC method. The proposed method was validated with respect to linearity, accuracy, precision and robustness. The method was successfully applied to the estimation of alprazolam and mebeverine in marketed formulations. Statistical analysis showed that the method is repeatable, selective, and precise.

A simple and accurate method for the analysis of ibuprofen (IBU) and famotidine (FAM) in their combined dosage form was developed using second order derivative spectrophotometery. IBU and FAM were quantified using second derivative responses at 272.8 nm and 290 nm in the spectra of their solutions in methanol. The calibration curves were linear in the concentration range of 100–600 μg/mL for IBU and 5–25 μg/mL for FAM. The method was validated and found to be accurate and precise. Developed method was successfully applied for the estimation of IBU and FAM in their combined dosage form.

A simple, sensitive, precise and stability indicating liquid chromatographic method has been developed for the estimation of desvenlafaxine succinate in pharmaceutical dosage form. A Hypersil C-18, 5 μm-column with a mobile phase containing 0.05 M potassium dihydrogen phosphate:methanol (60:40 v/v), pH 7, was used. The flow rate was 1.0 mL/min and effluents were monitored at 226 nm. The retention time of desvenlafaxine was 7.4 min and the method was linear in the range of 0.1-20 µg/mL. Desvenlafaxine stock solution was subjected to acid and alkali hydrolysis, chemical oxidation and dry heat degradation. The drug was found to be susceptible to base hydrolysis and developed method was found to give good separation between the pure drug and the degraded product. The method was successfully applied to the estimation of desvenlafaxine in tablet dosage forms.