A single RP-HPLC method is developed for estimation of isomeric impurities of vitamin D3 analogueCalcipotriol/Calcipotriene (Calci) and impurities of Betamethasone dipropionate (BD). The developed method is capable of separating impurities of Calci and BD, specifically pre-Calcipotriene (Pre-Calci) from other known and unknown impurities. Pre-Calci is isolated and is characterised using few analytical techniques. These impurities are separated using a RP-C18 150 × 4.6 mm, 2.7 µm column maintained at 50˚C. The mobile phase consisted of mixture of water, methanol, acetonitrile and tetrahydrofuran eluted in gradient mode. Detection was done at 264 nm and 240 nm for Calci and BD impurities respectively. The method can be used for determining quality of Calci and BD drugs and ointment based drug products. It is stability indicating related substance method for both the drugs and drug products.
Isosorbide 5-mononitrate (5-ISMN) has a direct relaxing effect on vascular smooth muscle. In the present study we developed matrix and reservoir-type transdermal patches of 5-ISMN. We investigated the usefulness of a new film-forming material isolated from the roots of Salacia macrosperma to serve as rate-controlling membrane for the reservoir-type patches. Matrix-type patches were formulated using polyvinyl chloride. Permeation studies through rat skin were conducted on both types of patches using Teflon cells. The mean +/- SD flux values from the matrix- and reservoir-type patches were 99.55 +/- 22.89 and 31.82 +/- 8.31 micrograms/cm2.hr, respectively.
In the recent past, delivery of therapeutic agents through the nasal route becoming a very attractive proposition, especially when rapid absorption and effects are required. The droplets size of a nasal spray dosage form is important for both efficacy and toxicity. In this study, an attempt was made to develop and validate a method to measure the droplets size distribution in Fluticasone nasal spray using Malvern spray tech coupled with automatic actuation station at various angles. Devices were actuated at the force of 6.0 kg, the velocity at 60 mm/s and rate of acceleration at 5000 mm/s 2. Data was collected for 150 ms at a height of 6.0 cm from the tip of the device. The method was evaluated for their precision, robustness and impact of different actuation angle on the formation of droplets size. The study revealed that changing the actuation angle from 0° to 45° had no significant impact on droplets size distribution of brand-B, whereas, the Dv (90) of brand-A significantly affected. The repeatability of the method was assessed from the percent standard deviation of six replicate measurements and was found to be 3.2, 5.3, 9.1 and 11.1 for Dv (10), Dv (50), Dv (90) and less than 10 µm respectively. Similarly, the robustness of the method was evaluated by changing velocity and acceleration. When the velocity changed to 55 and 65 from 60 mm/s the percent difference in their Dv (10), Dv (50) and Dv (90) was found to be-4.2,-7.6 and-11.4 for 55 mm/s and 0.4, 0.2 and 0.5 for 65 mm/s. When the acceleration changed to 4500 and 5500 from 5000 mm/s 2 the percent difference in their Dv (10), Dv (50) and Dv (90) was found to be-2.6,-1.7 and 0.1 for 4500 mm/s 2 and-3.3,-1.7 and 0.5 for 5500 mm/s 2. The results suggest that change in velocity and acceleration does not impact significantly on droplets size, thus ensures the robustness of the method. The method was applied to two commercially available nasal sprays labeled as Brand-A and Brand-B. The result has shown marginal differences in their Dv (10 and 50) but a significant difference observed in Dv (90) and Dv ˂10. The Dv (90) and Dv ˂10 of Brand-A and Brand-B was found to be 91.7; 0.8 and 66.9; 2.1 µm respectively. The data presented here suggest that the developed method is precise and robust can distinguish the droplets size change in the products. Hence, this can be adopted in the pharmaceutical industries to check the characteristics of the spray products. a.
Objective: The objectives of the present study were to develop and validate a mass compatible ultra-performance liquid chromatography (UPLC) method to quantify the impurities in fluticasone nasal spray, and to establish a suitable container-closure system for the formulation. Methods: A gradient method was optimized with a flow rate of 0.5 ml/min, detector wavelength-240 nm, run time-25 min and 0.1% Trifluoroacetic acid (TFA) in water as solvent A and Methanol as solvent B. Results: The developed method was linear over the range of 0.07-1.10 µg/ml for impurity-I, 0.16-2.47 µg/ml for impurity-II, 0.67-10.0 µg/ml for impurity-III, and 1.29-19.3 µg/ml for impurity-IV. The limit of quantification (LOQ) and limit of detection (LOD) were established as 0.07 and 0.02 µg/ml, 0.14 and 0.05 µg/ml, 0.59 and 0.19 µg/ml, 1.06 and 0.35 µg/ml for impurities I-IV respectively. The percent relative standard deviation (%RSD) of the replicate analysis for impurities I-IV, was within the acceptance criteria (0.4, 0.2, 0.3, and 0.1% respectively) that proved the precision of the method. The accuracy of the method was studied from 50%-150% of test concentration and the results ranged from 100.3% to 109.4%. The container-closure compatibility study revealed that the solution stored in the glass container system did not generate any additional peaks in the chromatogram. Conclusion: Hence, the developed method can be employed by quality testing laboratories to quantify impurities in fluticasone propionate nasal spray. The study also suggests that glass containers could serve as a compatible system for the storage of fluticasone propionate nasal solution.
Biorelevant dissolution media were designed and proposed based on physiological and physicochemical properties of the small intestine luminal contents in the fasted-and fed-state conditions. Biorelevant dissolution media have proved to be an excellent in vitro tool for predicting the in vivo performance of formulations in fasted-and fed-state conditions. Taurocholic acid and lecithin are surfactants used in biorelevant dissolution media to solubilize the drugs in dissolution media, which mimics the solubilization process of drugs in vivo.Preparation of biorelevant dissolution media is tedious and complex; it involves the emulsification of lecithin with methylene chloride followed by evaporation of methylene chloride under vacuum. In this work, an attempt was made to simplify biorelevant media preparation by applying high-speed stirring without methylene chloride. Biorelevant dissolution media prepared by the stirring method were clear and transparent. The performance of the media was compared by a dissolution study of two formulations in FaSSIF and FeSSIF media prepared by both the proposed method and a conventional method. The results of the dissolution test were comparable. The proposed method of biorelevant dissolution media preparation is simple, safe, reproducible, and less time consuming.
In the current study, the composition and process for preparing the nanosuspension of metaxalone (MX) has been optimized by using design of experiments (DOE). MX is skeletal muscle relaxant and belongs to BCS class II1 , the class wherein invivo drug dissolution is a rate-limiting step for drug absorption2 . High pressure homogenization (HPH) method was used to prepare the nanosuspension and Hydroxy propyl methyl cellulose (HPMC) and sodium lauryl sulfate (SLS) as surface stabilizers. For optimization studies three square (32 ) factorial design was used. For the composition optimization, concentration of the stabilizers and for process optimization homogenization time and pressure are used as independent variables. The dependent variables were particle size (PS), polydispersity index (PDI), zeta potential (ZP). The relationship between the dependent and independent variables was studied by response surface plots and contour plots. From the data it has been observed that 2.5 % HPMC, 0.5 % SLS were optimum concentrations and 1000 bar pressure, 120 minutes of homogenization were optimum process conditions producing least PS, PDI and high zeta potential. The optimized nano composition prepared by using optimum process conditions was observed to release more than 80 % within 30 minutes and found to be stable after 3 months of storage at room temperature. The solid state characterization (XRD, DSC) data of spray dried nanoparticles of the optimized composition has shown retention of drug crystallinity. IR has shown drug is compatible with the excipients used. SEM photograph has shown spherical drug nanoparticles. The optimization studies by applying the DOE resulted in considerable decrease in the experimentation work to achieve the stable nanosuspension with desired parameters such as PS, PDI and ZP.
A novel, sensitive, stability-indicating HPLC method has been developed for the quantitative estimation of Tolperisone-related impurities in both bulk drugs and pharmaceutical dosage forms. Effective chromatographic separation was achieved on a C18 stationary phase with a simple mobile phase combination delivered in a simple gradient programme, and quantitation was by ultraviolet detection at 254 nm. The mobile phase consisted of a buffer and acetonitrile delivered at a flow rate 1.0 ml/min. The buffer consisted of 0.01 M potassium dihydrogen phosphate with the pH adjusted to 8.0 by using diethylamine. In the developed HPLC method, the resolution between Tolperisone and its four potential impurities was found to be greater than 2.0. Regression analysis showed an R value (correlation coefficient) of greater than 0.999 for the Tolperisone impurities. This method was capable of detecting all four impurities of Tolperisone at a level of 0.19 μg/mL with respect to the test concentration of 1000 μg/mL for a 10 µl injection volume. The tablets were subjected to the stress conditions of hydrolysis, oxidation, photolysis, and thermal degradation. Considerable degradation was found to occur in base hydrolysis, water hydrolysis, and oxidation. The stress samples were assayed against a qualified reference standard and the mass balance was found to be close to 100%. The established method was validated and found to be linear, accurate, precise, specific, robust, and rugged.
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