Pharmaceutical Analysis Articles

CHROMATOGRAPHY- AN INTRODUCTION

About Authors:
Amit A. Patel
Seth G. L. Bihani S.D. College of Technical Education,
Institute of Pharmaceutical Sciences and Drug Research,
Sri Ganganagar, Rajasthan, INDIA.
amitpatelmx@gmail.com

ABSTRACT:
Chromatography may be defined as method of separating a mixture of components into individual component through equilibrium distribution  between two phases. chromatography is based on the differences in the rate at which components of mixture moves through a porous medium ( called stationary  phase ) under the influence of some solvent or gas ( called moving phase ). Graph showing detector response as a function of a time is called Chromatogram. The true separation of two consecutive peak on a chromatogram is measured by resolution.


X-ray APPLICATION

About Authors:
Nilesh Sovasia, Prof.Sanjeev Thacker, Arshad Hala
Seth G.L.Bihani S.D.College Of Technical Education,
Institute Of Pharmaceutical Science & Drug Research,
Sri Ganganagar, Rajasthan, India
*nilesh.sovasia@yahoo.com

ABSTRACT
X-rays have a smaller wavelength than visible light, they have higher energy. With their higher energy, X-rays can penetrate matter more easily than can visible light. Their ability to penetrate matter depends on the density of the matter, and thus X-rays provide a powerful tool in medicine for mapping internal structures of the human body.

H-NMR SPECTROSCOPY: AN INTRODUCTION

About Authors:
Arshad Hala*, Prof. Rajesh Dholpuria, Nilesh sovasia
Seth G. L. Bihani S. D. College Of Technical Education,
Institute Of Pharmaceutical Sciences & Drug Research,
Gaganpath, Sri Ganganagar, Rajasthan 335001
*Arshad_hala@yahoo.com

ABSTRACT:
Over the past fifty years nuclear magnetic resonance spectroscopy, commonly referred to as NMR, has become the preeminent technique for determining the structure of organic compounds. Nuclear Magnetic Resonance (NMR) spectroscopy is an analytical chemistry technique used in quality control and research for determining the content and purity of a sample as well as its molecular structure. For example, NMR can quantitatively analyze mixtures containing known compounds. For unknown compounds, NMR can either be used to match against spectral libraries or to infer the basic structure directly. Once the basic structure is known, NMR can be used to determine molecular conformation in solution as well as studying physical properties at the molecular level such as conformational exchange, phase changes, solubility, and diffusion.Of all the spectroscopic methods, it is the only one for which a complete analysis and interpretation of the entire spectrum is normally expected. Although larger amounts of sample are needed than for mass spectroscopy, NMR is non-destructive, and with modern instruments good data may be obtained from samples weighing less than a milligram. To be successful in using NMR as an analytical tool, it is necessary to understand the physical principles on which the methods are based.

Thermogravimetry

About Authors:
Jatin  Patel*
Seth G.L. Bihani S.D. College of Technical Education,
Institute of Pharmaceutical Sciences and Drug Research,
Sri Ganganagar, Rajasthan, INDIA
*Patelj313@yahoo.com

ABSTRACT:
Thermogravimetry
is a branch of physical chemistry, materials research, and thermal analysis. It is based on continuous recording of mass changes of a sample of material, as a function of a combination of temperature with time, and additionally of pressure and gas composition.

It includes different types of Thermogravimetric analysis. In this article types, Instrumentation, Procedure, Application are priscribed.

STABILITY-INDICATING RP- HPLC METHOD FOR ANALYSIS OF SITAGLIPTIN IN THE BULK DRUG AND IT’S PHARMACEUTICAL DOSAGE FORM

About Authors:
V.DEEPTHI *, POORNIMA.Y, DR.G.DEVALA RAO, T.SANDEEP REDDY
Department of Pharmaceutical Analysis,
K.V.S.R.Siddharthacollege of pharmaceutical sciences,
Vijayawada-520010, India.
*deepthi759@gmail.com

ABSTRACT
A novel stability-indicating RP-HPLC method has been develop and validated for quantitative analysis of Sitagliptin in the bulk drug and in its pharmaceutical dosage forms using Hypersil–BDS- C18 column (250x4.6mmi.d, 5µ particle size) with 10mM Phosphate buffer (PH-3.5): ACN 60:40%v/v as isocratic mobile phase enabled separation of the drug from its degradation products. UV detection was performed at 260 nm. The method was validated for linearity, accuracy (recovery), precision, sensitivity, ruggedness and robustness. The linearity of the method was excellent over the range 10–60μg/ml (correlation coefficient 0.999). The limits of detection and quantification were 0.21 and 0.640μg/ml, respectively. Recovery of Sitagliptinfrom the pharmaceutical dosage form ranged from 99.99 to 100.05%.

Sitagliptin was subjected to stress conditions (Hydrolysis (acid, base), oxidation,thermal and photo degradation) and the stressed samples were analysed by use of the method. Degradation was observed in acid, base, and 30% H2O2. The drug was stable under the other stress conditions investigated. The degradation products were well resolved from main peak. The forced degradation studies prove the stability indicating power of the method.

APPLICATION OF LC-MS

About Authors:
Jatin  Patel1*, Prof. Rajesh Kumar Dholpuria2, Dhiren Shah1
2(Professor, Head of Department of pharmacognosy),
1Seth G.L. Bihani S.D. College of Technical Education,
Institute of Pharmaceutical Sciences and Drug Research,
Sri Ganganagar, Rajasthan, INDIA
*Patelj313@yahoo.com

ABSTRACT:
Liquid chromatography is a fundamental separation technique in the life sciences and related fields of chemistry. Unlike gas chromatography, which is unsuitable for nonvolatile and thermally fragile molecules, liquid chromatography can safely separate a very wide range of organic compounds, from small-molecule drug metabolites to peptides and proteins. Traditional detectors for liquid chromatography include refractive index, electrochemical, fluorescence, and ultraviolet-visible (UV-Vis) detectors. Some of these generate two- dimensional data; that is, data representing signal strength as a function of time. Others, including fluorescence and diode- array UV-Vis detectors, generate three-dimensional data. Three-dimensional data include not only signal strength but spectral data for each point in time. Mass spectrometers also generate three- dimensional data. In addition to signal strength, they generate mass spectral data that can provide valuable information about the molecular weight, structure, identity, quantity, and purity of a sample. Mass spectral data add specificity that increases confidence in the results of both qualitative and quantitative analyses. For most compounds, a mass spectrometer is more sensitive and far more specific than all other LC detectors. It can analyze compounds that lack a suitable chromophore. It can also identify components in unresolved chromatographic peaks, reducing the need for perfect chromatography. Mass spectral data complements data from other LC detectors. While two compounds may have similar UV spectra or similar mass spectra, it is uncommon for them to have both. The two orthogonal sets of data can be used to confidently identify, confirm, and quantify compounds.

ANALYSIS OF SAMPLES BY TECHNIQUE OF GAS CHROMATOGRAPHY

About Authors:
Kapil Sharma*, Priyanka sharma
*Yaresun Pharmaceutical Pvt Ltd, Jaipur, India
*pharma_kapil@rediffmail.com

INTRODUCTION
Gas chromatography is a widely used technique for the separation of gaseous and volatile sub which are difficult to separate.The primary limit of s technique is that sample must be capable of being volatilized without undergoing decomposition because of this this technique is replaced by H.P.L.C.It is similar to column chromatography except that the gas is used as the mobile phase instead of the liquid.Here gas as a mobile phase or moving phase is passed through a column a column containing liquid adsorbent coated on inert solid support ,thus the adsorption or partition is possible.Gas solid chromatography(G.S.C) based upon the selective adsorption on solid,so the component of  mixture distributes them selves between the gas phase and adsorbent and the separation is due to adsorptive properties.where as Gas liquid chromatography (G.L.C) is based upon partition between Gas and immobile liquid coated on solid,.so the component of  mixture distributes them selves between the gas phase and liquid adsorbent coated on solid and the separation is due to partition properties1.

ANALYTICAL METHOD DEVELOPMENT AND VALIDATION FOR ESTIMATION OF CLOPIDOGREL BY DERIVATIVE SPECTROSCOPY (FOURTH ORDER)

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
Clopidogrel bisulfate is an inhibitor of adenosine diphosphate (ADP)-induced platelet aggregation acting by direct inhibition of ADP binding to its receptor and of the subsequent ADP-mediated activation of the glycoprotein GPIIb/IIIa complex. Objective of the present study is to develop a simple, sensitive, accurate, precise and rapid derivative spectrophotometric method for the estimation of clopidogrel in pure form. For the estimation of clopidogrel, solvent system employed was 0.1 N HCl and wavelength of detection (λdet) was 284.3 nm for fourth order derivative spectroscopy. The linearity was obtained in the range 42 – 336 µg/ml. The limit of detection is 6.7 µg/ml and limit of quantification was fund to be 20.4 µg/ml. 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 claim, thus suggesting the validity of the method and non-interference of formulation excipients in the estimation. Fourth order derivative spectroscopic method is simple, rapid and reproducible and further it can be used for the analysis.

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.


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 (λdet) 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.

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