Pharmaceutical Analysis Articles

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24 October 2012

ANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF CANDESARTAN CILEXETIL BY CHROMATOGRAPHIC TECHNIQUE (RP-HPLC).

About Authors:
Gunjan Kalyani*, Vishal S. Deshmukh, Pranita Kashyap, Ram D. Bawankar, Yogesh Vaishnav, Deepak Biswas
Shri Rawatpura Sarkar Institute of Pharmacy,
Behind power grid, Kumhari, Durg, Chhattisgarh
*kalyani.gunjan@yahoo.in

Abstract:
A simple, rapid and precise and accurate RP-HPLC method was developed for the estimation of candesartan. The method involves a simple technique using Irbesartan as internal standard. HPLC separation was achieved using C18 Intersil column (256 x 4.6 id) with an isocratic mobile phase composed of selected methanol: 10 mM Phosphate buffer [75:25 % v/v. pH 3.0] at a flow rate of 1.0 mL/min with UV detection was performed at 256 nm. The retention time of candesartan and internal standard was found to be 1.96 and 3.33 min respectively. The assay was validated for the parameters like accuracy, precision, robustness and system suitability parameters. The method was validated over a linear test concentration range of 80 - 120%. The recovery of the method was in between 99.0 - 101.0%. The proposed method was found to be accurate, precise, selective and rapid and it can be useful in the routine analysis for the determination of candesartan cilexetil in pharmaceutical dosage form.

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23 October 2012

ANALYTICAL METHOD DEVELOPMENT AND VALIDATION FOR THE ESTIMATION OF SALMETEROL BY UV SPECTROSCOPY

About Authors:
Gunjan Kalyani^*, Vishal S. Deshmukh, Pranita Kashyap, Yogesh Vaishnav, Ajit Kumar Pandey
Shri Rawatpura Sarkar Institute of Pharmacy,
Kumhari, Durg, Chhattisgarh.
kalyani.gunjan@yahoo.in, rvg_54767@yahoo.co.in*

Abstract:
The IUPAC Name of Salmeterol is (RS)-2-(hydroxymethyl)-4-{1-hydroxy-2-[6-(4-phenylbutoxy) hexylamino]ethyl}phenol. Salmeterol is a prescription drug that is used for treating airway spasms in people with asthma or chronic obstructive pulmonary disease (COPD). By relaxing the muscles around the airways to allow more air into and out of the lungs, the medication can help prevent asthma attacks from occurring.Salmeterol comes in the form of an inhalation powder and is generally used twice a day. Present research work deals with UV spectrophotometric method for the estimation of salmeterol in pure form. For the estimation of salmeterol, solvent system employed was ethanol and wavelength of detection (λ_det) was 252 nm. The linearity was obtained in the range 6 – 14 µg/ml, with a regression coefficient, R²= 0.999. The LOD & LOQ were found to be 4.99 µg/ml and 14.24 µg/ml respectively. Obtained results showed that there is minimum intra day and inter day variation. The developed method was validated and recovery studies were also carried out. Sample recovery using the above method was in good agreement with their respective labeled claims, thus suggesting the validity of the method and non-interference of formulation excipients in the estimation.
19 October 2012

UV- SPECTROPHOTOMETRIC METHOD DEVELOPMENT FOR THE DETERMENATION OF PARACETAMOL AND DROTAVERINE HYDROCHLORIDE IN COMBINATION TABLET DOSAGE FORM BY SIMULTANEOUS EQUATIONS METHOD

About Authors:
Rambabu.CH*, V. V. V. S. P. Apparao, Miss. M. Muthulakshmi, V. Ananth.
aPG-Student, Department Of Pharmaceutical Analysis,
KMCH College of Pharmacy,
Kalapatti Road, Coimbatore– 641 048, INDIA.
*ramgepharma@gmail.com

ABSTRACT:
At present, simultaneous determination of drugs in the combination dosage forms has been enjoying renaissance in the field of pharmaceutical analysis. Paracetamol, a classical antipyretic in combination with a novel antispasmodic drug, drotaverine hydrochloride provides a synergistic effect in the treatment of spasms. From the reviewed literature, it was simultaneous uv-spectrophotometric methods have not yet been developed for the determination and quantification of paracetamol and drotaverine hydrochloride. The λmax of paracetamol is 257 nm and that of drotaverine hydrochloride were scanned and found to be 308 nm, 352 nm. Both paracetamol and drotaverine hydrochloride were found to have significant absorbance of the λmax of each other and total absorbance was equal to the sum of the absorbance of paracetamol and drotaverine hydrochloride individually measured. So the present study involves the uv-spectrophotometric method development for the simultaneous determination of paracetamol and drotaverine hydrochloride by using simultaneous equations method. The mean % recoveries from this method were found to be 100.76% and 100.17% for paracetamol and drotaverine hydrochloride respectively proving that the method is accurate.
18 October 2012

ESTIMATION OF TEMOZOLOMIDE BY USING RP-HPLC IN ITS PHARMACEUTICAL DOSAGE FORM

About Authors:
Segu Sairam*, Mulla Mahaboob Basha, S Ananda Thangadurai, V Kranthi kumar
Swamy vivekanandha college of pharmacy, dept. Of pharmaceutical analysis,
Elayampalayam, tiruchengode – 637205.
*Sairampharma2020@gmail.com

ABSTRACT
A simple, sensitive and specific method reverse phase - high performance liquid chromatography (RP-HPLC) have been developed and validated for the estimation of Temozolomide in its Pharmaceutical dosage form.
Estimation of Temozolomide by using RP-HPLC coupled with UV
An isocraticREVERSE PHASE - HIGH PERFORMANCE LIQUID CHROMATOGRAPHY method was developed and validated for the estimation of Temozolomide in its Pharmaceutical dosage forms. The separation of the analytes was performed on aDevelosil ODS MG.5 (150×4.6mm),5µm, with mobile phase containing (0.5% w/v glacial acetic acid) named as Solution-A : Methanol [90 : 10, v / v] was used. The flow rate was 1 ml min^-1 and separation was monitored by UV detection at 254 nm. Chromatogram showed peak at a retention time of 7.306 ± 0.009 min. validation of the method for linearity and range, intra-day and inter-day precision, accuracy, specificity, recovery, ruggedness, robustness and limits of detection and quantification were obtained as 0.598 µg / ml and 1.81 µg / ml respectively. The calibration plot was linear from 20-60 µg ml^-1and the correlation coefficient was 0.999.The proposed method is fast, accurate and precise for the quantitative determination of Temozolomide capsules.

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11 October 2012

SIMULTANEOUS DETERMINATION OF IMIDAZOLE IN 2 METHYL IMIDAZOLE BY REVERSE PHASE LIQUID CHROMATOGRAPHY

About Authors:
Chandorkar J.G.
Head, Analytical development laboratory
Indofil Industries Limited
Thane.
jchandorkar-icc@modi.com

Abstract-
2 methyl Imidazole is the active raw material in the manufacturing of Micanazole Nitrate, Ketokenazole type Active pharma ceuticals. Imidazole is the Impurity which get form during manufacturing of 2Methyl Imidazole.
The Proposed Method is to determine the Impurity as well as Content in 2 Methyl Imidazole.
9 October 2012

SIMULTANEOUS ESTIMATION OF SILDINAFIL CITRATE AND DAPOXETINE HYDROCHLORIDE FROM COMBINED PHARMACEUTICAL FORMULATION USING A VALIDATED RAPID RP-HPLC METHOD

About Authors:
Nirav D.Langhneja^1*, Tushar Vaja¹, Dr. Vijay K. Parmar²
¹M.Pharm, Department of Pharmaceutical Sciences,
²Associate Professor, Department of Pharmaceutical Sciences,
Sardar Patel University,
Vallabh Vidyanagar-388120, Gujarat.
*laghnejanirav@gmail.com

INTRODUCTION
Sildenafil citrate 1-[[3-(6,7-Dihydro -1-methyl- 7-oxo-3-propyl -1H-pyrazolo [4,3-d] pyrimidin-5-yl) -4-ethoxyphenyl]sulphonyl]-4-methyl piperazine citrate and it is a popularly known as Viagra .It is a compound of the pyrazolo-pyrimidinyl-methyl piperazine class, and is used to treat male erectile dysfunction (Boolell.M et.al 1996, Morales. A, et.al 1998). It is a selective inhibitor of cyclic guanosine monophosphate (cGMP)-specific phosphodiesterase type 5 inhibitor. The structural formulae is C22H30N6O4S. It is an ampholyte with pKa value 4 (pirydinium ion) and 8.8 (benzimidazole). Sildenafil citrate is twice as soluble in methanol than in water. Its solubility decreases with pH up to 9 when it starts to increase again. Sildenafil citrate could be determined by several analytical techniques, Densitometry, spectrophotometry, colorimetry, HPLC, GC-MS, MEKC and capillary electrophoresis.
27 September 2012

ANALYSIS BY INSTRUMENTAL ANALYTICAL METHODS

About Authors:
Kapil Sharma^*1, Subhash Gupta²
¹Yaresun Pharmaceutical Pvt. Ltd.,India.
²Oasis test house ltd.jaipur-302006,rajasthan,india.
*pharma_kapil@rediffmail.com

INTRODUCTION
Most of the manufacturing industries rely upon both qualitative and quantitative chemical analysis to ensure that the raw material used meet certain specification, and also to check quality of the final product. The unwanted compound may be harmful to manufacturing process or may appear as a harmful impurity in the final product.¹

A quantitative analysis is performed to establish the proportion of the essential component in the raw material. The final manufactured product is analyzed to ensure that its essential component is present within a predetermined range of composition and impurities do not exceed certain specified limit.
23 September 2012

ANALYTICAL METHOD DEVELOPMENT AND VALIDATION FOR ESTIMATION OF IRBESARTAN BY DERIVATIVE SPECTROSCOPY (FIRST ORDER)

About Authors:
Gunjan Kalyani^*1, Vishal S. Deshmukh¹, Pranita Kashyap¹, Yogesh Vaishnav¹, Ram D. Bawankar
¹Shri Rawatpura Sarkar Institute of Pharmacy,
Kumhari, Durg, Chhattisgarh
*kalyani.gunjan@yahoo.in

Abstract
Irbesartan is chemically 2-butyl-3-({4-[2-(2H-1,2,3,4-tetrazol-5-yl) phenyl] phenyl} methyl) -1,3-diazaspiro [4.4] non-1-en-4-one. Irbesartan is an Angiotensin II receptor antagonist effective in the treatment of Hypertension. It is also effective in the treatment of High blood pressure. It is also effective when used alone or in combination with other drugs. Objective of the present study is to develop a simple, sensitive, accurate, precise and rapid first order derivative spectrophotometric method for the estimation of irbesartan in pure form. For the estimation of irbesartan, solvent system employed was 50% v/v aqueous ethanol and wavelength of detection (λ_det) was 237 nm. The linearity was obtained in the range 8 – 18 µg/ml, with a regression coefficient, R²= 1. The LOD & LOQ were found to be 0.5 µg/ml and 1.63 µg/ml respectively. Obtained results showed that there is minimum intra day and inter day variation. The developed method was validated and recovery studies were also carried out. Sample recovery using the above method was in good agreement with their respective labeled claims, thus suggesting the validity of the method and non-interference of formulation excipients in the estimation. First order derivative spectroscopy method is simple, rapid and reproducible and further it can be used for the analysis.
14 September 2012

METHOD DEVELOPMENT AND ITS VALIDATION FOR ESTIMATION OF DEFLAZACORT IN TABLET DOSAGE FORM BY UV SPECTROPHOTOMETRY

About Authors:
Kapil Sharma^*1, Subhash Gupta², Priyanka Sharma¹
¹Yaresun Pharmaceutical Pvt. Ltd.,India.
²Oasis test house ltd.
jaipur-302006,rajasthan,india.
*pharma_kapil@rediffmail.com

ABSTRACT
This paper describe a simple, precise and economical spectrophotometric method for the quantitative determination of Deflazacort(DFCT) in tablet dosage form. Method is based on the estimation of DFCT in aqueous acetonitrileat 246 nm. Beer’s law was obeyed in the concentration range of 4-14 µg/ml. The accuracy of the method was assessed by recovery studies and was found to be 99.38±0.15 for DFCT. Results of the analysis were validated statistically so that it can be used for routine analysis of DFCT in tablet dosage form.
4 September 2012

GC-MS ANALYSIS OF ACALYPHA INDICA LINN

About Author:
Manisha Singh
Sagar Institute of Pharmacy & Technology,
Gandhi nagar, Bhopal (M.P.)
manishamasih85@gmail.com

Abstract
Acalypha indica Linn. consists of dried herb of Acalypha indica Linn. belonging to familyEuphorbiaceae. Within the Euphorbiaceae family, Acalypha indica is one of the biggest and most diverse, with nearly 450 species. Two thirds of its species are found in America, 19 of them in Venezuala, they are mainly used as ornamental, but with the rising of traditional medicine, these species are given medical properties painkillers, laxatives, anti-inflammatory and many others.The GC-MS analysis of methanol and acetone (70 : 30) extract prepared from the whole plant of Acalypha indica linn. revealed the presence of different phytochemicals.