Volume 10 (1), 2012

Improved and Rapid HPLC-PDA Method for Identification and Quantification of Swertiamarin in the Aerial Parts of Enicostemma Axillare
Virendra Singh Rana, Tushar Dhanani and Satyanshu Kumar

A simple, improved, rapid and precise, reverse phase high performance liquid chromatography-photo diode array (HPLC-PDA) method has been developed and validated for the separation, identification and quantification of swertiamarin in aerial parts of Enicostemma axillare. The highest (38.12±1.74%) amount of swertiamarin was found in cold water and the lowest amount (20.13±0.84%) in hot water extracts obtained by using two different solvents. The separation of swertiamarin was achieved on a C18 column using the solvent system consisting of a mixture of methanol-water (1:1) as a mobile phase in a gradient flow elution mode followed by UV detection at 238 nm. The highest amount of swertiamarin was detected at 238 nm instead of detection at 227 nm and 254 nm. The developed method was validated using International Conference on Harmonisation (ICH) guidelines. Calibration curves offered good linear regression (r2>0.998) within the test ranges. In intraday assay, the maximum relative standard deviation (RSD; %) values were found to be 0.12, 0.1 and 1.59 for low (6 μg/mL), medium (20 μg/ mL and high (60 μg/mL) concentrations of swertiamarin. In interday assay, the maximum RSD (%) values were found to be 2.68, 2.71 and 2.88 for low, medium and high concentrations, respectively. Limit of detection (LOD) and limit of quantification (LOQ) were calculated to be 4 μg/mL and 6 μg/mL whereas analytical recovery ranged from 95.80%–101.76%.

Keywords: Gentianaceae, Enicostemma axillare, Swertiamarin, HPLC-PDA

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Development and Validation of LC Method for the Simultaneous Estimation of Rosiglitazone Maleate and Glimepiride in Pharmaceutical Dosage Form
Shweta Shashikat Havele and Sunil Rajaram Dhaneshwar

A simple, precise and accurate high performance liquid chromatography (HPLC) method was developed for simultaneous quantitative determination of rosiglitazone maleate and glimepiride in pure forms and in pharmaceutical formulation. The separation was achieved by C18 column using methanol:20 mM ammonium dihydrogen phosphate [78:22 (v/v); pH 3.85] as mobile phase at a flow rate of 1 mL/min and detection at 240 nm. Separation was complete in less than 10 min. Linearity, accuracy and precision were found to be acceptable over the ranges 0.8–4.0 μg/mL for rosiglitazone maleate and 0.4–2.0 μg/mL for glimepiride. This method was found to be specific, reproducible, precise and accurate. Due to its simplicity and accuracy the method is particularly suitable for routine pharmaceutical quality control.

Keywords: HPLC, Rosiglitazone maleate, Glimepiride, Multicomponent formulation

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RP-UPLC Method Development and Validation for the Determination of Nateglinide in Bulk Drug and Pharmaceutical Formulations: A Quality by Design Approach
Cijo Madathil Xavier, Kanakapura Basavaiah, Pavagada Jaganathamurthi Ramesh, Kanakapura Basavaiah Vinay and Hosakere Doddarevanna Revanasiddappa

Quality by design (QbD) is a systematic process to build quality into a product from the inception to final output. QbD requires a thorough understanding of a product and its process of manufacture, necessitating an investment in time and resources upfront in the discovery and development of a product. For QbD, the product and process knowledge base must include an understanding of variability in raw materials, the relationship between a process and product's critical quality attributes (CQAs), and the association between CQAs and a product's clinical properties. Here, a QbD approach to method development and validation is presented on nateglinide (NTG), an antidiabetic drug. To facilitate studies investigating the determination of NTG in bulk drug and its pharmaceutical formulations, we developed and validated a rapid ultra performance liquid chromatography (UPLC) method for determination of NTG. The validated limit of quantitation (LOQ) of 0.06 μg mL^-1 and limit of detection (LOD) of 0.02 μg mL^-1 are low enough to allow determination of low concentrations of the drug. NTG showed no degradation at different stress conditions. The relative standard deviation (RSD) percentage for robustness and ruggedness were observed within the range of 0.1 and 1.74. The calibration was linear in the range of 0.06–250 μg mL^-1. The proposed method was compared with a pharmacopoeial reference method and found to give equivalent result. The proposed method can be used for routine analysis in quality control laboratories for its bulk and formulated product and this is the first reported UPLC method for the assay determination of NTG.

Keywords: UPLC, Nateglinide, QBD, Validation, Degradation

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Formulation and Evaluation of Fast Disintegrating Rizatriptan Benzoate Sublingual Tablets
Balusu Haarika and Prabhakar Reddy Veerareddy

Rizatriptan benzoate is a potent and selective 5-HTIB/ID receptor agonist and is effective for the treatment of acute migraine. Sublingual formulation has the advantage of offering fast relief from migraine due to faster drug delivery. The present study involves the formulation and evaluation of fast disintegrating sublingual tablets of rizatriptan benzoate to produce intended effects. The sublingual rizatriptan benzoate tablets were prepared by the method of direct compression. The superdisintegrants used were sodium starch glycolate, cross carmellose sodium and cross povidone. The powder flow properties of all formulations were evaluated for diameter, thickness, weight variation, hardness, friability, wetting time, water absorption ratio, drug content, in vitro and in vivo disintegration time as well as in vitro release and were found to be satisfactory. The optimised formulation containing cross povidone disintegrated very fast and in vitro drug release was very high. The optimised formulation was characterised by scanning electron microscopy (SEM), differential scanning calorimetry (DSC), powder x-ray diffraction (PXRD) and fourier transform infrared spectroscopy (FTIR). Based on disintegration and dissolution studies, the optimised formulation was also evaluated for in vivo release studies using rabbit model. The peak serum concentration (C_max), half time needed for item to decay (T_½), time for maximum plasma concentration (T_max) and area under curve (AUC) were calculated. T_max for rizatriptan tablet was faster in sublingual route when compared to oral route. Rizatriptan tablet by sublingual route in rabbit shows effective therapeutic Cmax when compared to clinical dose and it is a promising alternative to oral administration route in acute management of migraine.

Keywords: Rizatriptan benzoate, Fast disintegrating sublingual tablets, Pharmacokinetics, LCMS/MS

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Comparative Study of Mucoadhesive Polymers Carbopol 974P and Sodium Carboxymethyl Cellulose for Single Unit Dosage of Imatinib Mesylate
Vinod Kombath Ravindran, Santosh Vasa, Sandhya Subadhra, David Banji, Otilia Banji and Yamsani Madhusudhan Rao

The aim of this study was to design and develop controlled release Imatinib mesylate (IM) oral dosage form by fabricating gastroretentive mucoadhessive tablet which can retain the drug in the stomach for prolonged duration and to achieve therapeutic levels over an extended period of time for the treatment of myelogenous leukemia (CML) and gastro intestinal stromal tumor (GIST). Single unit formulations containing carbopol 974P or sodium carboxy methyl cellulose (MC) which helps the drug in adhering to the gastric mucosa for an extended period of time were formulated and evaluated. Gastroretentive tablets of IM were prepared by direct compression. The results obtained showed no physicochemical incompatibility between the drug and other excipients used in the formulations. The prepared tablets were evaluated by different parameters such as thickness, weight variation, hardness, content uniformity, swelling index and mucoadhesive strength. Indigenously fabricated assembly was used to measure the bioadhesive strength of the mucoadhesive tablets, and goat gastric mucosa was used as a model tissue. Bioadhesive strength increased with increasing the amounts of carbopol 974P and sodium CMC in the formulations. The physicochemical compatibility of the drug with other excipients used in the formulations was studied by FTIR analysis. The tablets were also evaluated for in vitro drug release in 0.1N HCl for 12 h in USP Type II dissolution apparatus. In order to determine the mode of release, the data was fitted into various kinetic models and the optimised formulation followed Korsmeyer peppas model and the ‘n’ value was greater than one indicated super case II mechanism of drug release. The radiographic pictures of the rabbits confirm the in vivo mucoadhesion in the stomach for 6 h.

Keywords: Gastroretentive, Mucoadhesive, Imatinib mesylate, Radiography

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Age and Gender-Based Utilisation Pattern of Antidiabetic Drugs in Ajman, United Arab Emirates
Lisha Jenny John, Mohammed Arifulla, Jayadevan Sreedharan, Jayakumary Muttappallymyalil, Rajdeep Das, Jenny John and Altaf Basha

Diabetes is a chronic multi-system metabolic disease associated with significant morbidity, mortality and cost to the society. Socio-demographic factors like age and gender may affect prescribing pattern. The objective of the study was to evaluate the drug usage pattern of antidiabetic drugs in different age groups and gender. A cross sectional survey of all prescriptions of patients with diabetes attending the Outpatient Department (OPD) of Internal Medicine of Gulf Medical College Hospital and Research Centre, Ajman, United Arab Emirates was conducted for three months. The socio-demographic and drug information for each patient was obtained using a questionnaire. A total of 132 prescriptions were included in this survey whereby 54.8% of patients were males and 45.2% were females. The mean age of patients with diabetes was 54.09±10.24 years. Hundred twenty eight prescriptions were for patients with type 2 diabetes. Metformin alone and in combinations were the commonly prescribed antidiabetic drug. Insulin prescription was noted in 14 patients (type 1 and 2 diabetes), the commonest being human insulin. Metformin combinations were most commonly prescribed in both genders. For patients below 45 years and those between 45–60 years of age, metformin combinations were the commonest prescribed, while among patients above 60 years of age sulfonylureas were the most commonly prescribed. The utilisation pattern of antidiabetic drugs varied among different age groups and gender. Metformin alone and combinations with newer antidiabetic medications were commonly utilised.

Keywords: Utilisation pattern, Antidiabetic drugs, Diabetes, United Arab Emirates

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