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  • 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.

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  • DEVELOPMENT AND VALIDATION OF QUETIAPINE BY HPTLC METHOD

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

    Abstract
    The aim of the present work is to develop validated HPTLC method which determines stress stability and concentration of Quetiapine and its formulation as per ICH guidelines. Separation was performed using Camag Linomat V semi Automated sample applicator with TLC Scanner III. HPTLC analytical measurement and separation were performed using Stationary Phase consisting of TLC plates (Merck) pre coated with silica gel 60F254 on Aluminum Sheets was used. Mobile phase comprising of Methanol: Toluene (7:3 v/v) was used. All the system suitability parameter was found within the range. Area under curve was measured at 235nm. The method was extensively validated for specificity, linearity, accuracy, precision, recovery, limit of quantitation and detection. The proposed method can be used for routine analysis of Quetiapine in quality control laboratories.

  • 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.

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  • 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.

  • 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.

  • 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-1 and 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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  • 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.

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

    About Authors:
    Nirav D.Langhneja1*,
    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.

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