Stability Indicating HPTLC Method for Simultaneous Determination of Amlodipine Besylate and Lisinopril in Combined Dose Tablet Formulation

A combined dose tablet formulation containing Amlodipine besylate and Lisinopril is used for the treatment of essential hypertension. The present study reports development and validation of stability indicating high performance thin layer chromatographic method for simultaneous estimation of these drugs in combined dose tablet formulation. The two drugs were satisfactorily resolved on aluminum plates precoated with silica gel 60F254 using n-butanol : methanol: ammonia (4:4:1 v/v/v) as mobile phase. The Rf value for lisinopril and amlodipine besylate were 0.27±0.02 and 0.62±0.02, respectively. Densitometric evaluation of the separated bands was performed at 215nm. The calibration curves for lisinopril and amlodipine besylate were found to be linear in the concentration range of 1000-6000ng/band. The method was validated as per ICH guidelines for accuracy, precision, robustness, specificity, limit of detection and limit of quantitation. Statistical analysis proves that the method is suitable for simultaneous analysis of Lisinopril and Amlodipine besylate in pharmaceutical formulation without any interference from the excipients/degradant. The developed method offers several advantages such as sensitive, rapid, cost effective and less time consuming as compared to the reported methods. As the method could effectively separate the drugs from its degradation products, it can be employed as a stability indicating method.

Formulation & Evaluation of Effervescent Tablet of Verapamil Hydrochloride

The chief aim of the present investigation is to study the Formulation & Evaluation of Effervescent Tablet of Verapamil Hydrochloride. The floating tablets of verapamil hydrochloride were prepared by direct compression technique. For each tablet formulation, drug, HPMC-K15M, karaya gum, sodium bicarbonate, and diluents were blended homogeneously for 10 min followed by addition of magnesium stearate. The total weight of each tablet was 300 mg. The amount of karaya gum used was in the range of 40–90 mg, whereas HPMC was used in the range of 20-40 mg. The powder mixture was further mixed for 5 min in a mortar. The resultant mixture was compressed into tablets using a Rimek rotary tablet machine. After preparation, the formulations were evaluated by various parameters. The friability of the tablet formulation varied between 0.3 ± 0.0063 to 0.59 ± 0.0076%. The weight variation of prepared tablet formulation complies with USP limits. The thickness was found to be in the range of 4.1 ± 0.48 to 4.2 ± 0.76 mm. The assay for drug content varied between 96.53 ± 0.36 to 102.03 ± 0.52%. The B1, B5, B6, B9, and B10 exhibited more than 75% drug release at 12 h. The B1 exhibited a maximum of 30 % drug release in the 1st hour and constant release for almost up to 12 h. B8 showed the least drug release among all other formulations; this may be due to the formation of a thick gel barrier on the tablet. Tablets were prepared by direct compression. Technological characteristics of floating tablets were within the Pharmacopoeial limit. Tablets floated for more than 8 h. Complete swelling was achieved by the end of 8 h, so percent swelling was determined at the end of 8 h for all the developed formulations.

QUANTIFICATION OF BILASTINE AND MONTELUKAST COMBINATION IN FORMULATIONS UTILIZING LIQUID CHROMATOGRAPHY: STABILITY STUDIES

Objective: We have developed a “stability-indicating RP-HPLC” procedure for the Bilastine (BLS) and montelukast (MTL) analysis of tablets. Methods: The quantification of BLS and MTL combination was implemented utilising a Waters column (C18, 5 μm, 250 mm and 4.6 mm). Isocratic mobile phase had 60% volume KH2PO4 of 0.1M strength with pH 4.2 units and 40% volume methanol at a flow with 1.0 ml/min speed. UV detection at 232 nm was done to examine BLS and MTL. Stability experiments of BLS and MTL under distinctive environments of stress were also performed. Results: The BLS and MTL were eluted at 1.810 min and 2.551 min, respectively. The responses were found to be linear for the concentration ranges of 10-30 µg/ml (BLS) and 5-15 µg/ml (MTL). Percent comparative standard deviance for precision was 0.331% (BLS) and 0.486% (MTL). Percent assay for accuracy was 98.96% (BLS) and 99.00% (MTL). The detection limit and quantitation limit measures for BLS were 0.018 µg/ml and 0.059 µg/ml, respectively, while for MTL it was 0.024 µg/ml and 0.081 µg/ml, respectively. Robustness studies authorized that the method is robust with percent comparative standard deviance of a highest 1.950%. Conclusion: The developed “stability-indicating RP-HPLC” procedure for the BLS and MTL analysis is simple, sensitive, precise, specific and robust, making it appropriate to the assessment of BLS and MTL in a tablet formulation.

New stability indicating RP-HPLC-PDA method for determination of mifepristone in bulk and tablet formulation

Background Mifepristone is progestational and glucocorticoid hormone antagonist. The objective of this study is to develop simple and economical stability indicating RP-HPLC method for the determination of mifepristone in bulk and tablet formulation. Result The chromatographic separation was achieved on Qualisil BDS C8 column with mobile phase containing of mixture of Buffer (Potassium dihydrogen ortho phosphate, pH to 3.0 with ortho phosphoric acid) and Organic Solvent (Acetonitrile) 60:40 v/v pumped at flow rate 0.6 mL min−1. The detection of elute was performed using PDA detector at 305 nm. Mifepristone was eluted at 8.67 min. According to international conference on harmonization Q2(R1) guideline, method was validated and shows satisfactory results for accuracy, precision, linearity, ruggedness, robustness, detection limit, quantitation limit. The method indicated to be linear in the series of concentration 3–18 µg mL−1, and correlation coefficient was 0.9997. In acidic, basic, oxidative, thermal, photolytic forced degradation conditions, the peak of degradation product was clearly and well separated from drug peak without any interference in quantitative analysis. This represents stability indicating nature of established method. Conclusion The established RP-HPLC method is simple, accurate, specific, precise, robust, rugged, sensitive, and economical in nature which can be utilized for routine analysis of mifepristone in bulk and pharmaceutical formulation.

Formulation and Development of Metoprolol Succinate Sustained Release Matrix tablet using Remusatia vivipara tubers mucilage

The purpose of this research was to formulate and evaluate sustained release tablet by using novel polymer Remusatia vivipara tubers mucilage. Currently natural gums and mucilages are being used extensively comparable to synthetic drug release modifiers. Natural plant materials possess various advantages. These are very cheap, biocompatible, biodegradable and free from side effects. In present research Metoprolol succinate matrix tablets were prepared by using Remusatia vivipara tubers mucilage. For the formulation of sustained release matrix tablets, direct compression method was used. The formulated matrix tablets were then evaluated for thickness, diameter, hardness, weight variation, friability, drug content, swelling index, in-vitro drug release and stability studies. The formulated sustained release tablet passed all tests required. The dissolution profile of prepared tablets showed sustained release of drug up to 11 hours compared to the reference tablet formulation PROLOMET XI 100. Drug release data were then fitted in to release kinetic models such as zero order kinetic, first order kinetic, Higuchi model and Korsmeyer-Peppas model to study the release pattern of drug from each formulation. The prepared sustained release tablet formulation was compared with marketed formulation (reference formulation) for drug release study and factor f1 (difference factor) and f2 (similarity factor) were determined. From this study it can be concluded that as the concentration of Remusatia vivipara mucilage increases, there is decrease in the rate of drug release from the formulation. The best formulation was found to be F3 which consists of 20% Remusatia vivipara mucilage but did not give comparable drug release profile to the reference formulation with factor f1 69.4 % and f2 34.8%. But it can be said that Remusatia vivipara gum mucilage can be used in tablet formulation to give sustained release effect up to 10 hours or in combination with other natural gum mucilage it may enhance the release retardant effect of drug up to or more than 20 hrs. The release kinetic study showed that the prepared sustained release tablet formulation shows anomalous (non-fickian) diffusion pattern and follows both diffusion controlled and swelling controlled mechanisms for drug release.

Development and Validation of RP-HPLC method for the Estimation of Ritonavir in API and tablet Formulation

A Reverse Phase High Performance Liquid Chromatographic method has been developed and validated for estimation of Ritonavir in API and Tablet formulation. The chromatographic separation was carried out using ZOROBAX Bonus-RP C-18 column (250 x 4.6mm, 5µm) as stationary phase and Methanol: Acetonitrile: 0.1% Trifluoroacetic acid water (81:9:10) as mobile phase at 1.0 ml/min flow rate and detection was carried out at 250 nm. The method was validated accordance to the Guidelines of International Council for Harmonization (ICH). Ritonavir have linearity in the concentration range of 50-150µg/ml with correlation coefficient (r2=1) respectively. Ritonavir eluted at 3.05 min respectively. The method is sensitive, precise and accurate. So, the method can be successfully applied for the routine analysis of Ritonavir in pharmaceutical formulations.

Simultaneous analysis of eprosartan and hydrochlorothiazide in tablet formulation by High- Performance thin layer chromatography with ultraviolet absorption densitometry

A new, simple, accurate, and precise high-performance thin-layer chromatographic method has been established for simultaneous analysis of Eprosartan and Hydrochlorothiazide from a tablet formulation. Standard and sample solutions of Eprosartan and Hydrochlorothiazide were applied to precoated 250 μm layer of silica gel G 60 F and the plates were developed with Chloroform: Acetonitrile: Glacial Acetic Acid (7:3:1,v/v/v) as mobile phase. Detection and evaluation of densitograms was performed densitometrically at 254 nm. The linear range was 200-700 ng/band with the retention factors of Eprosartan and Hydrochlorothiazide were 0.26± 0.02 and 0.44±0.02, respectively. The method was validated and successfully used for analysis of the drugs in tablets.