Stability-Indicating TLC-Densitometric and HPLC Methods for Simultaneous Determination of Teneligliptin and Pioglitazone in Pharmaceutical Dosage Forms with Eco-Friendly Assessment.

The combination of teneligliptin hydrobromide hydrate and pioglitazone hydrochloride in pharmaceutical formulations has improved type 2 diabetes management. Two chromatographic methods TLC-densitometry and RP-HPLC were developed for simultaneous quantification of teneligliptin hydrobromide hydrate and pioglitazone hydrochloride in pharmaceutical formulations, ensuring accuracy and stability assessment. The TLC method uses a mobile phase of methanol, toluene, ethyl acetate and triethylamine (1:7:2:0.1, v/v/v/v) on TLC silica gel plates, scanned at 268 nm. The RP-HPLC method employs isocratic elution with acetonitrile and sodium acetate buffer (adjust pH 3.6 with glacial acetic acid, 60:40 v/v) on a shimpack C18 column (250 × 4.6 mm i.d., 5 µm), detected at 235 nm. Both methods offer high accuracy and reliability, making them valuable for pharmaceutical quality control. Additionally, an environmental impact assessment was conducted using eco-scale, Analytical Greenness Metric Approach, Green Analytical Procedure Index, and national environmental method index to evaluate solvent consumption, waste generation and energy usage. Statistical comparisons (t-tests and F-tests) validate the outcomes of both methods, ensuring their effectiveness in drug formulation analysis. These methods can enhance pharmaceutical quality control while fulfilling environmental responsibilities.

Development and Validation of HPLC Analytical Method for Chlorantraniliprole in Bulk and in the Formulation.

BACKGROUND: Chlorantraniliprole is widely used as a pesticide. It is only soluble in dimethyl formamide. However, most of the reported methods used acetonitrile and other solvents. AIM: To develop rapid, accurate, precise, and sensitive HPLC method for chlorantraniliprole. MATERIALS AND METHODS: 10 µG/mL of chlorantraniliprole containing solution was injected into the HPLC system and run in different solvent systems. 10 µG/mL solutions of chlorantraniprole was injected in a column with 20 µL microsyringe. The chromatogram was run for appropriate minutes with mobile phase water. The flow rate was set to 1 mL/min and detection was carried out at wavelength 270 nm. The method is validated by measuring the limit of quantitation, limit of detection, repeatability, intraday precision, inter-day precision, and accuracy. Analysis of marketed formulation, bringle, and tomato for chlorantraniprole content was also made for the developed analytical method. RESULTS: There was linearity of chlorantraniliprole for calibration curve in between 1 and 5 µG/mL concentration. The perfect sharp peak observed in water at a retention time of 6.28 min. The limit of detection and the limit of quantitation were 0.0050 µG/mL and 0.0152 µG/mL, respectively. The study reported 99.55% repeatability, 99.49% intraday precision, 99.65% interday precision, and 99.27% accuracy. CONCLUSION: The rapid, accurate, precise, and sensitive HPLC method for the detection of chlorantraniliprole using dimethyl formamide was developed.

Nuts and Bolts of Oil and Temperature in Topical Preparations of Salicylic Acid.

BACKGROUND: Traditional formulations of salicylic acid in ointment bases have disadvantages of being greasy and irritant due to free crystals. AIM: To explore the method for selection of oils and their ratio for topical preparation on the basis of equilibrium solubility study of salicylic acid and to evaluate temperature effect. MATERIALS AND METHODS: Scanning and calibration curve of salicylic acid in methanol were developed. Among available oils, those that had no interference of absorbance of salicylic acid were short-listed for screening purpose. Selections of oils were carried out on the basis of equilibrium solubility study. Compatibility study was made by Fourier Transform Infra-Red spectroscopy analysis. Primitive study of oil mixtures was done. Selections of the ratio of oils were carried out on basis of constrained simplex-centroid design. RESULTS: Salicylic acid had shown linearity in the range of 15-65 µg/mL in methanol at wavelength maximum (300 nm). From the equilibrium solubility study, Parker Neem® Oil (11.81 ± 0.5 mg/g), Isopropyl Myristate (11.29 ± 0.04 mg/g), Mogra Oil (9.62 ± 0.94 mg/g) were selected. The study possessed the same main Fourier transform infra-red peaks of salicylic acid in the salicylic acid-oils physical mixture. 58.64% Parker Neem® oil and 41.36% isopropyl myristate mixture was selected as optimized batch with the desirability of 0.391. CONCLUSION: The oils mixture could be selected for topical preparation of salicylic acid like paste, cream, ointment etc.

Association of Permeability and Lipid Content of Membrane.

BACKGROUND: Rat skin and goat cul de sac are mostly used in optimization of formulations as the model of human skin and cul de sac. AIM: To explore the correlation between lipid content of rat skin and goat cul de sac and permeability. MATERIALS AND METHODS: Find out wavelength maximum for Sapat plus malam®, Ciplox eye ointment® and chloramphenicol eye caps and the standard curve was also derived. In vitro studies using Cellophane® membrane and ex vivo studies using rat skin or goat cul de sac of the formulations. Permeability coefficient, % dislodgeable dose, lag time, diffusion parameter, and partition coefficient were found for both studies after six and a half hours of penetration studies. Student's unpaired t-test with equal variance was used to find any statistically significant difference in the ex vivo and in vitro diffusion transport studies at 95% level of confidence. RESULTS: Permeability coefficient of Sapat plus malam®, Ciplox eye ointment® and chloramphenicol eye caps were 0.000316 ± 0.0000625, 0.00416 ± 0.0001, 0.0034 ± 0.00004 for Cellophane® membrane and 0.0001 ± 0.000001, 0.002254 ± 0.0002, 0.00303 ± 0.0001 for ex vivo membrane in cm2/min, respectively. For all three formulations, there were calculated t values which were higher than tabulated t values at 95% of confidence level (P<0.05). CONCLUSION: Cellophane® membrane shows a better diffusion than rat skin or goat cul de sac. In the optimization of formulation, only Cellophane® membrane is advisable to use.

Emulsion of Chloramphenicol: an Overwhelming Approach for Ocular Delivery.

BACKGROUND: Ophthalmic formulations of chloramphenicol have poor bioavailability of chloramphenicol in the ocular cavity. AIM: The present study aimed at exploring the impact of different oil mixtures in the form of emulsion on the permeability of chloramphenicol after ocular application. MATERIALS AND METHODS: Selection of oil mixture and ratio of the components was made by an equilibrium solubility method. An emulsifier was chosen according to its emulsification properties. A constrained simplex centroid design was used for the assessment of the emulsion development. Emulsions were evaluated for physicochemical properties; zone of inhibition, in-vitro diffusion and ex-vivo local accumulation of chloramphenicol. Validation of the design using check-point batch and reduced polynomial equations were also developed. Optimization of the emulsion was developed by software Design® expert 6.0.8. Assessment of the osmolarity, ocular irritation, sterility testing and isotonicity of optimized batch were also made. RESULTS: Parker Neem®, olive and peppermint oils were selected as an oil phase in the ratio 63.64:20.2:16.16. PEG-400 was selected as an emulsifier according to a pseudo-ternary phase diagram. Constrained simplex-centroid design was applied in the range of 25-39% water, 55-69% PEG-400, 5-19% optimized oil mixture, and 1% chloramphenicol. Unpaired Student's t-test showed for in-vitro and ex-vivo studies that there was a significant difference between the optimized batch of emulsion and Chloramphenicol eye caps (a commercial product) according to both were equally safe. CONCLUSION: The optimized batch of an emulsion of chloramphenicol was found to be as safe as and more effective than Chloramphenicol eye caps.