Pharmaceutical Analysis Articles

About Authors:
Kapil Sharma¹*, Subhash Gupta ², Yogesh Sharma¹
1 Yaresun Pharmaceuticals Pvt. Ltd.Jaipur - 302006, Rajasthan, India.
2 Oasis test house ltd.jaipur-302006,
Rajasthan, India.

METHOD DEVELOPMENT AND ITS VALIDATION FOR ESTIMATION OF TORSEMIDE IN TABLET DOSAGE FORM BY RP-HPLC AND UV SPECTROPHOTOMETRY AND COMPARISON OF TWO DEVELOPED METHODS BY USING t-TEST

ABSTRACT
One HPLC and one UV spectrophotometric method have been developed for the determination of torsemide (TRS) in tablet dosage form. The first method is based on determinetion of TRS in tablet dosage form by RP- HPLC method.  Chromatgraphy was carried out on a nucleosil C-18,250 x 4.6 mm column using a mixture of phosphate buffer and methanol  (50:50 v/v)  as the mobile phase at a flow rate of 1.3 ml/min.  Run time was 15 min.  Detection was done at 288 nm and retention time of the drug was 7.05 min.  This method produced linear responses in the concentration range 60-140  µg/ml of torsemide. The accuracy of the method was assessed by recovery studies and was found to be 99.90± 0.41 for torsemide.  The second method is based on the estimation of torsemide in tablet dosage form by UV spectrophotometry using 50% v/v methanol in distilled water.  Beer’s law obeyed over the concentration range 2-26 µg/ml at 288 nm with apparent molar absorptivity of 1.26 x 10⁴.  Both developed methods were found to be applicable for routine analysis of drug in tablet dosage form. The result of the analysis were validated statistically.The results were compared obtained from UV spectrophotometry and HPLC.

About Authors:
Rajkumar Bolledula*, Priyanka.Mare¹, Sunanda.Mare²
*Department of pharmaceutical analysis, Assistant professor in MITS college of pharmacy, H.No.41-64-s, saibabanagar, Kurnool-518004, A.P, India.
1.Department of pharmaceutics, Assistant professor, Mits college of pharmacy, Block .no.mc2/2, singareni colony, tekulapally,yellandu,khammam-507123,A.P,India
2.Department of pharmacology, J.K.K.Natarajan college of pharmacy, Salem, Tamil Nadu

ABSTRACT
This article describes the quantitative determination of percentage of drug concentration in pure and in formulated pharmaceutical dosage forms by using RP-HPLC. Procedure does not require prior separation of components from the sample.The mobile phase consists of methanol-water (80:20 v/v) for RP-HPLC with injection volume of 20μl.The RP-HPLC method was developed on a C-8 (150x4.6mm) column with detection carried out by variable wavelength detector at 209nm and 220 nm for ramipril, cardace, odopril respectively…Thus the Rt values obtained for different dosage forms are 1.59,1.44,1.34,1.35…..respectively with the concentration of 100% for pure drug and 97.54%,91.03%,65.76%.......respectively.

About Author:
Sugumaran M., T. Vetrichelvan
Department of Pharmaceutical Chemistry,
Adhiparasakthi College of Pharmacy,
Melmaruvathur - 603 319, Tamilnadu , India

Abstract
High performance thin layer chromatographic finger print parameters had been developed for  Piper betle leaf oilisolated from karpoori, sirugamani and vellaikodi variety available in tamilnadu to fix standards. At shorter wavelength (254 nm) resolution was better for, so, this wavelength can be taken for obtaining optimum HPTLC finger printing for  volatile oil of this medicinal plant leaves. As per the data,   Karpoori variety of piper betle leaf oil  only showed  presence of  eugenol content. So, essential oil obtained from this variety should be included in the commercial tooth paste to get  antimicrobial activity against dental pathogens when compared to other studied variety.

About Author:
Sharath Kumar Pallikonda*¹, Srikanth Subburu², Shanker Reddy Soma², Chandra Shekar Reddy^3
1,2Vathsalya College Of Pharmacy,
Bhongir, Dist: Andhra Pradesh, India - 508 116

Abstract
A simple, sensitive, rapid, robust and reproducible method for the determination of Quetiapine fumarate in bulk and pharmaceutical formulation (Tablets) was developed using reverse phase high performance liquid chromatographic method (RP-HPLC). The RP-HPLC analysis was performed isocratically on XTERRA C18 (4.6X150mm), analytical column using a mobile phase consisting of ortho phosphorus buffer and acetonitirle in the Ratio of 60:40v/v, with a flow rate of 0.6ml/min. The analyte was monitored with UV detector at 290nm. The developed method Quetiapine fumarate elutes at a run time of 10 min. The proposed method is having linearity in the concentration range from 40 to 80 μg/mL of Quetiapine fumarate. The present method was validated with respect to system suitability, linearity, precision, limit of detection (LOD) and limit of quantification (LOQ), accuracy (recovery), ruggedness, and robustness. The proposed method can be readily utilized for bulk drug and pharmaceutical formulations.

About Author:
B. Raj kumar*, M. Priyanka¹, K. V. Subrahmanyam², Syed Mujtaba Ahmed³, Ch. RakeshReddy¹, R. Prem Sagar¹
*Department of Pharmaceutical Analysis
Mits College of Pharmacy, kodad, Nalgonda
1. Department of Pharmaceutics
Mits College of Pharmacy, Kodad, Nalgonda
2. Department of Pharmaceutical Analysis
PIPS, Suryapet, Nalgonda
3. Department of Pharmaceutical chemistry
Netaji college of Pharmacy, Choutuppal, Nalgonda

Abstract:
The present work deals with the studies carried out on the development, optimization and validation of RP-HPLC and HPTLC methods for the simultaneous estimation of Telmisartan and Ramipril in combined dosage form. Market is folded with combination of drugs in various dosage forms. The multi-components formulations have gained a lot of importance now days due to greater patient acceptability, increased potency, multiple action, fewer side effects and quicker reliefs. For simultaneous estimation of drugs present in multi-component dosage form, High Pressure Liquid Chromatography (HPLC) and High Pressure Thin Layer Chromatography (HPTLC) methods are considered to be most suitable since it is extremely precise, accurate, sensitive, linear and rapid.  The literature survey carried out and it revealed that several analytical methods have been reported for estimation of these drugs as individual or in combination with other drugs. So the objective of the work is to develop HPLC and HPTLC methods for simultaneous estimation of drugs in multi-component dosage form for which no analytical method has been previously reported. Hence, present study have been planned to develop a specific, precise, accurate, linear, simple and rapid HPLC and HPTLC methods for simultaneous estimation of Telmisartan and Ramipril in tablet dosage form.

About Authors:
Sukanto Paul, Krishan R Bhadu
Department of Quality Assurance, School of Pharmaceutical Sciences,
Jaipur National University,
Jagatpura, Jaipur-302025,
Rajasthan, India.

ABSTRACT
A validated reverse phase high performance liquid chromatography method has been developed for the simultaneous determination of Tirofiban hydrochloride in pure and marketed formulation. Chromatography was carried out on a BDS Hypersil C18 (4.6 mm × 250 mm, 5 μm) using Buffer: Acetonitrile in the ratio of 80:20 (v/v) as the mobile phase at a flow rate of 1.5 mL/min and eluents were monitored at 274 nm using UV detector at ambient temperature.  The average retention time of Tirofiban was found to be 9.124 min. The method was validated for linearity, precision, accuracy, specificity, robustness and solution stability. The calibration curve was linear (R²≥0.9999) over the range of 12.5-75 μg/mL.Limit of detection (LOD) and Limit of quantitation (LOQ) were 0.11 μg/mL and 0.33 μg/mL respectively. This method can be successfully employed for the quantitative analysis of Tirofiban hydrochloride in bulk drugs and formulations.

About Author: Rajesh Nuni
Department of Pharmaceutical Analysis,
Vels School of Pharmaceutical Sciences,
Vels University, Pallavaram,
Chennai, Tamilnadu, India

Abstract
A reverse phase HPLC method is developed for the determination of Sumatriptan and naproxen in pharmaceutical dosage forms. Chromatography was carried out on a C8 column [4.6 x 150mm, 3.5mm, Make: XTerra] using a mixture of potassiumdi hydrogen ortho phosphate buffer and acetonitrile (50:50 v/v) as the mobile phase at a flow rate of 0.7ml/min. Detection was carried out at 285 nm. The retention time of the drug Naproxen and sumatriptan was 2.24 minand 5.871 min. The method produced linear responses in the concentration range of 60 to 100μg/ml of Sumatriptan and naproxen. The LOD values for HPLC method for naproxen and sumatriptan were found to be 3.20 and 3.36 ng/ml. The LOQ for Naproxn and Sumatriptan were foud to be 9.86 and 9.90 ng/ml respectively. The method was found to be applicable for determination of the drug in tablets.

About Author: Mr. Mahesh W. Thube*, Dr. Sadhana R.Shahi, Mr. Abhay Padalkar
Mr. Mahesh W. Thube*: Department of Pharmaceutics,
Government College of Pharmacy, Aurangabad - 431 005, Maharashtra, India
Dr. Sadhana R. Shahi: Assisstant Professor, Govt. College of Pharmacy, Aurangabad, Department of Pharmaceutics.

Abstract
Ion exchange resin (IER) is high molecular weight polyelectrolyte having charged functional site. IER are chemically vinyl, divinyl benzene and polystyrene copolymers. IER in past years have received extensive attention by pharmaceutical industry due to their versatile application. Previously IER were mainly used for water purification only but recently they have been studied for Novel Drug Delivery System. IER are mainly used for taste masking but, they also possess modifying release properties. The IER are complexed with drug to form resinates by batch process or column process. If necessary the resinates are coated with polymeric material by microencapsulation technique. Coated resinates acts as a controllable rate limiting factor for exchange of ions and also for exchange of drug, thus, modifying the release of drugs. The review article highlights the application of sustained and controlled release resinate for the development of various drug delivery system.

About Authors: Manoj Kumar Jadia1*, Dr. U. L. Narayan2
1. Department of Pharmaceutical Chemistry,
Indira Gandhi institute of Pharmaceautical Sciences,
IRC village, Bhubaneswar, Odhisa, India
2. Principal, Department of Pharmaceutical Chemistry,
Indira Gandhi institute of Pharmaceautical Sciences,
IRC village, Bhubaneswar, Odhisa, India

Abstract
The two methods are described for the simultaneous determination of Paracetamol and Etodolac in binary mixture. The first method was based on UV-spectrophotometric determination of both of the drugs, using simultaneous equation method. It involves absorbance measurement at 256.0 nm (λmax of Paracetamol) and 226.0 nm (λmax of Etodolac) in methanol; linearity was obtained in the range of 5 – 25 μg.mL-1 for both the drugs. The second method was based on HPLC separation of the two drugs in reverse phase mode using Promosil C18 column. Linearity was obtained in the concentration range of 30-70μg.mL-1 for Paracetamol and 20-60 μg.mL-1 for Etodolac. The LOD and LOQ value of UV-Spectrophotometric determination was found to be 167.43 ng mL-1, 507.37 ng mL-1  and for HPLC determination was found to be 1653.12 ng mL-1, 5009.48 ng mL-1.Both these methods have beensuccessively applied to pharmaceutical formulation and were validated according to ICH guidelines.