Pharmaceutical Analysis Articles

  • PharmaTutor
    30 December 2012

    AN OVERVIEW OF LIQUID CHROMATOGRAPHY COUPLED WITH TANDEM MASS SPECTROSCOPY (LC-MS/MS)

    About Authors:
    *S.B.Muthu Vadivel, R.Suresh Kumar, A.Tamil Selvan, R.Suthakaran
    Department of Pharmaceutical Analysis and Quality Assurance
    Teegala Ram Reddy College of Pharmacy
    Saroor nagar, Meerpet, Hyderabad – 97.
    *muthuvadivelanalyst@gmail.com

    Abstract
    Mass spectrometry has been applied to almost every area of research being pursued today. Studies of diverse subjects, such as cancer research, identification of drugs, forensic analysis, atmospheric end-water environmental analysis, combustion, and lasers have benefited from mass spectrometry. In some of these studies, the mass spectrometer is used both as a chemical reactor and as an analytical instrument. Because of these diverse applications, no person or group can completely review the field of mass spectroscopy. This chapter discusses instrumental designs and techniques, ionization processes, ion–molecule reactions, high-temperature systems, and sampling of reactive species. Any tandem mass spectroscopy has four basic components: (I) a system by which the sample to be studied is introduced into the instrument, (II) an ion source where ions that are characteristic of the sample are produced, (III) an analyzer region where the ion beam is sorted into its various mass-to-charge ratios, and (IV) a detector system where the separated ion beams are collected and by some method, rendered observable.

  • 28 December 2012
    INSTRUMENTATION OF ESR SPECTROSCOPY

    About Authors:
    Lila dhar*1,Surender Jalandra
    1Seth G. L. Bihani S. D. College Of Technical Education,
    Institute Of Pharmaceutical Sciences & Drug Research,
    Gaganpath, Sri Ganganagar, Rajasthan 335001
    *ldbudania@gmail.com

    ABSTRACT
    Electron paramagnetic resonance spectroscopy (EPR) is a powerful tool for investigating paramagnetic species, including organic radicals, inorganic radicals, and triplet states. The basic principles behind EPR are very similar to the more ubiquitous nuclear magnetic resonance spectroscopy (NMR), except that EPR focuses on the interaction of an external magnetic field with the unpaired electron(s) in a molecule, rather than the nuclei of individual atoms. EPR has been used to investigate kinetics, mechanisms, and structures of paramagnetic species and along with general chemistry and physics, has applications in biochemistry, polymer science, and geosciences. The use of cavity stabilised Impatt diode oscillators for ESR spectroscopy is discussed in different experimental conditions: i.e. as microwave sources in reflection cavity homodyne spectrometers, and as marginal oscillators in which the oscillator cavity (a TE011 cylindrical cavity) is the observing cavity. The sensitivity of this second configuration has been theoretically evaluated for the case in which the Impatt itself is used as a detecting element and in which an external detector is used. For each situation the sensitivity has been measured with a DPPH sample at various power levels giving a sensitivity which is comparable with the best commercial units.

  • 11 December 2012
    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.

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  • 10 December 2012
    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.

  • 7 December 2012
    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.

  • 30 November 2012
    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.

  • 29 November 2012
    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.

  • 11 November 2012
    STABILITY INDICATING HPTLC METHOD DEVELOPMENT AND VALIDATION FOR CINACALCET HYDROCHLORIDE API

    About Authors:
    Gautam Kumar
    SRM college of pharmacy, SRM University
    Chennai 600 033.
    gautamsinghsrmcp@gmail.com

    Abstract
    The aim of the present work to develop validated RP-HPLC method which determines stress stability and concentration of Cinacalcet hydrochloride in synthetic mixture as per ICH guidelines. Separation was performed using Camag Linomat V semi Automated sample applicator with TLC Scanner III. Stationary Phase consisting of TLC plates (Merck) pre coated with silica gel 60F254 on Aluminum Sheets was used. Mobile phase comprising of Methanol: Water: Glacial acetic acid (5:5:0.2v/v/v) was used. All the system suitability parameter was found within the range. The method was extensively validated for specificity, linearity, accuracy, precision, recovery, limit of quantitation and detection. The Cinacalcet hydrochloride was found to be highly labile to alkaline and acid hydrolysis compared to oxidation. Chromatographic peak purity results indicated the absence of co-eluting peaks with the main peak of Cinacalcet, which demonstrated the specificity of assay method for estimation of Cinacalcet in presence of degradation products. The proposed method can be used for routine analysis of Cinacalcet in quality control laboratories.

  • 7 November 2012
    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.

  • 31 October 2012
    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.

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