Stability Indicating HPTLC Determination of Triamcinalone Acetonide in Bulk Drug and Sterile Injectable Suspension

Abstract

A sensitive, accurate, precise and stability indicating high-performance thin layer chromatographic method was developed and validated for analysis of triamcinalone acetonide (TRIA) in bulk drug and sterile injectable suspension. The method employed HPTLC aluminum precoated plates with silica gel 60F-254 as the stationary phase. The solvent system consisted of Toluene: ethyl acetate: ammonia solution (33:67:0.1 %v/v). This system was found to give compact bands for TRIA (R f value 0.38 ± 0.02). TRIA was subjected to acid, alkali and neutral hydrolysis, oxidation, sun light and dry heat treatment. The degraded products were well separated from the pure drug with notably different R f values. CAMAG semi-automatic HPTLC used for the analysis. Densitometric analysis of TRIA was carried out in the absorbance mode at 240 nm. The linear regression data for the calibration plots showed good linear relationship with correlation coefficient 0.9996 ±/ 0.001 in the concentration range of 100.0-2000.0 ng spot -1. The values of slope and intercept were 9.7841 and -86.13 respectively. The method was validated for precision, accuracy, robustness, and recovery. The limits of detection and quantitation were 33.0 and 100.0 ng spot -1 respectively. As the method could effectively separate the drug from its degradation products, it can be employed as a routine stability indicating assay method. suitable for routine determination of TRIA in bulk drug and in formulations. The proposed method was validated in compliance with ICH guidelines, 8,9 and its updated international convention. 10Experimental Materials TRIA bulk drug and its injectable suspension were given by Star drugs and research laboratories, Bangalore as a gift sample. Ethyl acetate, Toluene, methanol and ammonia solution (Qualigens Fine Chemicals, Mumbai) used were of analytical grade, CAMAG linomat IV sample applicator equipped with 100 ml Hamilton (USA) syringe, CAMAG twin trough glass chamber, CAMAG TLC scanner III densitometer, Cats 3 software. HPTLC instrumentationThe samples were applied in the form of bands on the plate, width 6 mm, and 10 mm from the bottom of the edge using a Merck precoated silica gel aluminium plate 60F-254 (20×10 cm with 0.2 mm thickness, E.Merck, Germany) with Linomat IV (Switzerland) sample applicator equipped with a 100µL Hamilton (USA) syringe. A constant application rate of 100 nL/s was employed and the standard, sample volume was 10 µL, the space between two bands were 7 mm and slit dimension was kept 5x0.45 mm micro and 5 mm sec -1 scanning speed was employed. The eluting solvent was consisted of Toluene: ethyl acetate: ammonia solution (33:67:0.1 % v/v). Linear ascending development was carried out in twin trough glass chamber (CAMAG) saturated with mobile phase. Previously the glass chamber was saturated with the help of filter paper and the optimized chamber saturation time was found to be 30 min at room temperature. The length of chromatogram run was appro ximately 80 mm. After the development the plates were dried in air w...

Reliable and Sensitive Stability Indicating – Liquid Chromatographic Method for Determination of Azilsartan Medoxomil and Characterization of Common Hydrolytic Degradation Product

“…[14][15][16][17][18][19][20][21][22][23] Degradation was induced at a concentration of 1000 µg/ml. At different time points, 0.5 ml of degraded solution was diluted with mobile phase to 10 ml(50 µg/ml), pH was adjusted between 3-4 with dil.…”