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The present work is aimed to develop a simple, sensitive, robust and reliable HPLC method for the estimation of irinotecan in the physiological media in order to assess the permeability profile of irinotecan, using the everted gut sac, in the presence of various P-gp modulators. Separation was achieved using, C18 column with mobile phase consisting of acetonitrile and 0.045 µM sodium dihydrogen phosphate dihydrate buffer containing ion pair agent heptane sulphonic acid sodium salt (0.0054 µM), pH 3. The fow rate was maintained at 1 ml/min and analysis was performed at 254.9 nm using PDA detector. Calibration data showed an excellent linear relationship between peak-area verses drug concentration (r², 0.9999). Linearity was found to be in the range of 0.060-10.0 µg/ml. Limits of detection and quantifcation were found to ~0.020 µg/ml and ~0.060 µg/ml, respectively. The developed method was found to be precise (RSD <1.5%, for repeatability and <2.55% for intermediate precision, acceptable ranges of precision), accurate (The recovered content of irinotecan in the presence of various P-gp modulators varied from 96.11-101.51%, within acceptable range, 80-120%), specifc and robust (% RSD <2). Developed method has been applied successfully for the evaluation of eleven P-gp modulators from diverse chemical class. [ABSTRACT FROM AUTHOR]

A sensitive, selective, precise, and stability-indicating, high-performance, thin-layer chromatographic (HPTLC) method for analysis of sertraline, both as a bulk drug and in house formulation, was developed and validated. The method employed thin-layer chromatographic (TLC) aluminium plates precoated with silica gel 60F-254 as the stationary phase. The solvent system consisted of Toulene/Ethyl acetate/Ammonia (1:5:0.1, v/v) as a mobile phase. The densitometric analysis were carried out at 273 nm using Camag TLC scanner which generated compact spots for SRT (Rf = 0.70 ± 0.02). The linear regression data for the calibration plots showed good linear relationship with r2 = 0.998 in the concentration range of 25–2000 ng spot−1. Sertraline was subjected to acid and alkali hydrolysis, oxidation, photodegradation, and dry heat treatment. Also, the degraded products were well separated from the pure drug. The method was validated for precision, accuracy, ruggedness, and recovery. As the method could effectively separate the drug from its degradation products, it can be employed as a stability indicating one. Moreover, the proposed HPTLC method was utilized to investigate the kinetics of acid and base degradation process. [ABSTRACT FROM AUTHOR]

Purpose: In this paper, simple, specific and accurate RP-HPLC method was developed in order to study decomposition of sertraline (SRT) under the hydrolytic stress conditions (acid, neutral, alkaline and oxidative). Materials and Methods: The best separation of SRT and its degradation products were achieved on reverse phase LiChoCART with Purospher (RP-18e) column. The mobile phase was composed of methanol/water (75:25, v/v). The detection wavelength was 273 nm. The method was validated and response was found to be linear in the drug concentration range of 10-200 µg ml-1 with correlation coefficient of 0.998. Results: The RSD values for intra- and inter-day precision were < 0.65 and < 0.72%, respectively. Employing RP-HPLC method, degradation products were detected in the exposed samples. Conclusion: It was found that the susceptibility of SRT to hydrolytic decomposition increased in following manner: Neutral condition < alkaline condition < acid condition < oxidative condition. [ABSTRACT FROM AUTHOR]

A stability-indicating high-performance thin-layer chromatographic (HPTLC) method was developed and validated for quantifying Itraconazole (Itz) in bulk drug, marketed formulation, and an in-house formulation comprised of lipidic-nano particle incorporated into vaginal gel. Aluminum plates precoated with silica gel 60 F-254 were used for TLC with Toulene:Ethyl acetate:Ammonia (1:5:0.1 v/v) as a mobile phase. The densitometric analysis was carried out at 266 nm using a Camag TLC scanner that generated compact spots for Itz (R f =0.77 ± 0.02). The regression analysis data for the calibration curve exhibited good linearity (r2 = 0.996 ± 0.0058). The LOD and LOQ values were found to be 14.29 ng spot−1 and 43.31 ng spot−1, respectively, while their recovery (99.65–100.23%) and precision (1.47%) were found to be satisfactory. Itraconazole was also subjected to forced stress conditions such as hydrolysis (acid and alkali), oxidation, dry and wet heat degradation, and photo degradation. The degradants were further characterized by NMR and Mass spectroscopy and compared with neat drug. Statistical analysis revealed that the developed method has potential for routine analysis of Itz in various formulations. It is well suited for quality control and study of pharmaceutical parameters such as release profile, loading, and entrapment in lipidic nanoparticle formulation. [ABSTRACT FROM AUTHOR]

A simple, sensitive, precise, and accurate stability-indicating high performance thin-layer chromatographic method for analysis of irinotecan both as bulk drug and in marketed injectables has been developed and validated as per ICH guidelines. Chromatographic separation was achieved on LiChrospher aluminum plates precoated with silica gel 60F254 as stationary phase. The solvent system consisted of acetone-ethyl acetate-acetic acid 8.5:1.5:0.1 (v/v/v) and this system was found to give compact spots for irinotecan at RF value of 0.31 ± 0.02. Densitometric analysis was performed in the absorbance at 366 nm. The linear regression analysis for the calibration plots showed good linear relationship with r2 = 0.9973 ± 0.0013 in the concentration range of 50-500 ng/spot. The method was validated for precision, accuracy, recovery, and specificity. The % recovery (94.63-101.40%) and precision (≤4.30) were found to be satisfactory. Irinotecan was subjected to acid and alkali hydrolysis, oxidation, thermal, and ultraviolet radiation treatments. All the peaks of degradation products were well resolved from the standard drug with significantly different retention factor (RF) values. Developed method effectively separated out the drug from its degradation products and hence can be used as stability-indicating method as well as in routine analysis of irinotecan. [ABSTRACT FROM AUTHOR]