Pharmaceutical Analysis Articles


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

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.

Analytical Method Development and Validation for Simultaneous Determination of Sumatriptan and Naproxen by RP - HPLC

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

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.

Review on Ion Exchange Resin: An Approach towards Sustained / Controlled Release Delivery System

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.

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.

UV - Spectrophotometric and RP - HPLC Method Developement for Simultaneous Determination of Paracetamol and Etodolac in Pharmaceutical Dosage Form

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

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.

Estimation of Olmesartan Medoxomil and Atorvastatin Calcium in Tablet Dosage Form by HPLC Method

About Authors: Venkata Suresh Babu Aluri*
Department of pharmaceutical Analysis,
Adhiparasakthi College of Pharmacy,
Melmarvathur, Kancheepuram District, Tamil Nadu - 603319 (INDIA)

Reference ID: PHARMATUTOR-ART-1077

A simple, specific, sensitive, rapid, precise and economical high performance liquid chromatography (HPLC) method has been developed for the estimation of Olmesartan medoxomil (OLM) and Atorvastatin calcium (ATC) in tablet dosage form by using acetonitrile- phosphate buffer pH 3.0 (40:60 v/v) as a solvent system. The method was carried out on a Phenomenex Gemini C18 (15 cm x 4.6 mm i.d., 5µm particle size) column, at flow rate 0.9 mL/min. Detection was carried out at 252 nm. The retention time of OLM and ATC was 3.19 and 4.63 min, respectively. The two drugs follow Beer-Lambert’s law over the concentration range of 8 – 40 µg/mL for OLM and 4 – 20 µg/mL for ATC. Validation of proposed method was carried out for its accuracy, precision, specificity and ruggedness according to ICH guidelines. The proposed method can be successfully applied in routine work for the determination of Olmesartan medoxomil and Atorvastatin calcium in combined dosage form.


About Author: V. Ranjith Kumar*, Chintalapti Sujitha
* Department of Pharmaceutical Analysis,
Priyadarshini college of Pharmaceutical Sciences,
Chowdaryguda, Narapalli, Ghatkesar (Mo),
RR-District-501301. AP-INDIA.

Reference ID: PHARMATUTOR-ART-1062

A simple, accurate, cost effective and reproducible spectrophotometric method has been developed for the estimation of Sitagliptine in bulk and pharmaceutical dosage form. Visible spectrophotometric method, which is based on measurement of absorption at maximum wavelength 540 nm. The accuracy of the methods was assessed by recovery studies and was found to be ranging from 99.5-101.5 .The developed method was validated with respect to linearity, accuracy (recovery), precision and specificity. Beers law was obeyed in the concentration range of 25-125 µg/ml having line equation y = 0.026x + 0.016 with correlation coefficient of 0.999. Results of the analysis were validated statistically and by recovery study.


1.     Research scholar of Jawaharlal Nehru Technological University, Department of Pharmaceutical Analysis, College of Pharmacy, Kakinada, Andhra Pradesh, India.  

Reference ID: PHARMATUTOR-ART-1042

This present study reports for the first time simultaneous quantitation of Amlodipine besylate and Atorvastatin calciumby HPTLC from a combined dosage form.
Methods: Chromatographic separation of the drugs were performed on aluminum plates precoated with silica gel 60 F254 used as stationary phase and the chromatogram was developed using Ethyl acetate: Methanol: Ammonia (7.5 : 2 : 0.5 %v/v/v) as mobile phase. Amlodipine besylate and Atorvastatin calcium showed Rf values 0.50 ±0.02 and 0.26 ±0.02 respectively. Densiometric analysis of both the drugs was carried out in the absorbance mode at 365 nm. The method has been successfully applied to tablets and was validated according to ICH Harmonized Tripartite guidelines.
Results: The linearity regression analysis for calibration showed 0.9983 (r2) and 0.9994 (r2) for amlodipine besylate and atorvastatin calcium with respect to peak area and height in the concentration range of 100-500ng/spot and 200-600ng/spot respectively.  The percentage recovery for amlodipine besylate was found to be 101.82 (at 50%), 99.12 (at 100%) and 101.41 (at 50%), 101.71 (at 100%) for atorvastatin calcium. The limit of detection was 30 ng/spot and    60 ng/spot for amlodipine besylate and atorvastatin calcium respectively. The limit of quantification was found to be 100 ng/spot and 200 ng/spot for amlodipine besylate and atorvastatin calcium respectively.
Conclusion: The developed TLC technique is precise, specific and accurate. It was concluded that the developed method offered several advantages such as rapid, cost effective, simple mobile phase and sample preparation steps and improved sensitivity made it specific, reliable and easily reproducible in any quality control set-up providing all the parameters are followed accurately for its intended use.


About Author: Amit Surani,
Dept. of Quality Assurance,

M.Pharm, Maliba College of Pharmacy, Surat
Gujarat Technical University

According to FDA, Process Analytical Technology (PAT) is a system for designing, analyzing, and controlling manufacturing process through timely measurements of critical quality and performance attributes of raw materials, in-process materials and processes with the goal of ensuring final product quality.
PAT involves the use of different technologies and tools to build quality into the products. Effective PAT implementation is based on detailed, science-based understanding of the physical, chemical and mechanical properties of all elements of the proposed drug product.
Pharmaceutical companies face many challenges while implementing PAT into their new and pre-existing manufacturing processes. This article discusses the challenges encountered by manufacturers and the benefits they can reap by successful implementation of PAT.

Chemistry of Tamsulosin HCl and Estimation of Tamsulosin HCl by high performance liquid chromatography.

About Authors: Kollu Varuni, B.pharm
Vathsalya college of pharmacy,
J.N.T.U University

Tamsulosin is a selective, potent and competitive a  1 – adrenoreceptor antagonist and has a greater affinity for these receptors, predominantly present in the human prostate. Literature survey reveals that several methods like HPLC,HPLC-MS and LC-MS were reported for the estimation of Tamsulosin hydrochloride in combination with other drugs as well as in biological fluids [1- 3]