Gas chromatographic techniques are ideal for by rnrj9uO

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									            RAJIV GANDHI UNIVERSITY OF HEALTH SCIENCES
                          BANGALORE, KARNATAKA
                                ANNEXURE-II


               PERFORMA FOR REGISTRATION OF SUBJECT FOR DISSERTATION



1.0 NAME OF THE CANDIDATE & ADDRESS      DATENDRA NATH TRIPATHI
                                         S/0 Mr. SURENDRA NATH TRIPATHI
                                         #HOUSE NO 365
                                          VILLAGE & POST – NEEWA,
                                          ALLAHABAD -211003,
                                          UTTAR PRADESH,


2.0 NAME OF THE INSTITUTION              AL-AMEEN COLLEGE OF PHARMACY,
                                         BANGALORE


3.0 COURSE OF STUDY & SUBJECT            M.PHARM ( Part- 1)
                                         PHARMACEUTICAL CHEMISTRY


4.0 DATE OF ADMISSION                    08-JULY-2010




5.0 TITLE OF THE TOPIC;

    “ESTIMATION OF RESIDUAL SOLVENTS IN HERBAL EXTRACT BY GAS CHROMATOGRAPHY
    USING PHARMACOPOEIAL AND VALIDATION METHOD”.
6.0 BRIEF RESUME OF THE INTENDED WORK;

    6.1; NEED OF STUDY;

    Organic volatile impurities are residual solvents that are used in or produced in the synthesis
    of drug substances or in excipients, or in the preparation of herbal formulations.

    The determination of residual solvents in the herbal extracts or formulations is known to be
    one of the most difficult and demanding analytical tasks in the pharmaceutical industry.

     The organic impurities may arise during the manufacture or storage of new substance. They
    may be identified or unidentified, volatile of non-volatile; include Starting material, by product,
    intermediate, degradation product reagents, ligands and catalysts.

    The estimation of residual solvents is considered as an important tool in the quality control of
    pharmaceutical.

    Gas chromatography is based on the volatilized sample transported by the carrier gas as the
    moving phase through the stationary phase of the column where separation takes place by the
    sorption/desorption process. Samples for gas chromatographic analysis are normally low
    molecular weight compounds that are volatile and stable at high temperature. In this respect,
    residual solvents in drug substances and drug products are suitable for gas chromatographic
    analysis. Chemical derivatives can also be formed to achieve volatility and thermal stability.

     Method validation was the process used to confirm that the analytical procedure employed for
    a specific test is suitable for its intended use. Results from method validation can be used to
    judge the quality, reliability and consistency of analytical results; it is an integral part of any
    good analytical practice.

      Analytical methods need to be validated or revalidated:

        before their introduction into routine use;
        whenever the conditions change for which the method has been validated (e.g., an
           instrument with different characteristics or samples with a different matrix); and
        Whenever the method is changed and the change is outside the original scope of the
           method.
7.0 7.1; LITERATURE SURVEY:

         C.C. Camarasu performed two static headspace gas chromatographic methods for
         residual solvent determination in pharmaceutical products have been developed, optimized
         and validated .The methods are sensitive (allowing detection limits of as low as 0.1 ppm for
         benzene), accurate and precise(1).

         S.B Puranik, Varun R Pawar, N. Lalitha, P.N. Sanjay Pai and G. K. Rao had been
         validated gas chromatographic method for estimation of residual solvents in intermediates
         and APIs. Acetone and IPA was found in impramine HCl, in colmipramine HCl only IPA
         was detected, ethyl acetate and toluene were detected in Doxepin HCl and Pargiverine
         HCl(2).

         Puranik SB, Sanjay Pai PN, Rao GK had been validated gas chromatographic method for
         estimation of residual solvents methanol and isopropyl alcohol in Momardica charentia,
         Morinda Citrifolia, Rosemary, Curcumin, Greentea, Gymnema, Phyllantus niruri(3).

         Biljana Nikolic, Vele Tesivic, Iris Dordevic, Milka Jadranin and others perpormed gas
         chromatography (GC) and gas chromatography–mass spectrometric (GC–MS) analysis for
         n-Alkanes in the needle waxes of Pinus heldreichii var.pancic(4)

         Yoko Uematse and coworkers had determined the low levels of methanol and ethanol in
         licorice extract by lagre volume injection head space gas chromatography (5).

         Chun-Di Hu , Yi-Zeng Liang , Fang-Qiu Guo had determined the essential oil composition
         from Osmanthus fragrans tea by GC-MS combined with a chemometric resolution
         method(6).

       Abhishek Gupta and coworker developed and validated the head space chromatographic
       method for the quantification of residual solvents present in arterolane maleate bulk drug
       through an understanding of the synthetic process, nature of solvents and nature of
       stationary phases of columns. The residual solvents pentane, ethanol, 2-methylpentane,
      n-heptane, 3-methylpentane, n-hexane,methylcyclopentane, cyclohexane, benzene and
       dichloromethane were determined(7).

         P N Sanjay Pai, B Balaphanisekhar, GK Rao, K Pasha had determined of methylene
         chloride as residual solvent was developed and validated on gas liquid chromatograph
         fitted with flame ionization detector in the marketed formulations of ciprofloxacin
         hydrochloride, norfloxacin, pefloxacin and ofloxacin(8).
     
          S J Wadher, Manisha Puranik, PG Yeole, CS Lokhande determined ethanol in
         Abhayarishta using gas liquid chromatography. Abhayarishta is a common ayurvedic
         preparation, belonging to asava and arista categories, generally prepared soaking the drug
         either in powder form or in the form of decoction ( Kasaya )(9)
      7.2; OBJECTIVE OF THE STUDY ;

           Residual solvents from the processes in the manufacturing of pharmaceuticals are
            hazardous and cause serious problems and must be removed.


          Gas chromatographic techniques are ideal for residual solvent analysis. They are
           selective for characterization of residual solvents and also sensitive to accurately
           determine these solvents in trace amounts, when present in pharmaceutical
           substances. Recognizing the need to control the presence of these solvents, which are
           likely to cause undesirable toxic effects.




8.0     MATERIAL AND METHODS;

        8.1 Source of data;
                 References from the library- Al- Ameen College of pharmacy, Bangalore.
                 www.google.com
                 www.sciencedirect.com
                 Instrument- Gas chromatography;
                 Phytochemistry journals
                 www.ijpsonline.com
                 Indian Journal of Chemistry
                 Indian Journal of Pharmaceutical Chemistry
                 Phytochemistry journals




        8.2) Method development;

             Analytical experiments will be planned and executed at Natural remedy Bangalore.
              The following instrument is proposed to be used for collection of data

                Head space gas chromatogram.
      8.3) Methods and instrumentation;

             The gas chromatography instrument use for the estimation of residual solvents in the
         herbal extracts.




      8.4) Methodology;

                   All experiments will be carried out in the Natural remedies Bangalore.


      8.5)   DOES THE STUDY REQUIRE ANY INVESTIGATION TO BE CONDUCTED
                                  ON PATIENTS OR ANIMALS?

                                         -NO-




      8.6)   HAS ETHICAL CLEARANCE BEEN OBTAINED FROM YOUR INSTITUTION IN
         CASE OF 8.5?

                             -      NOT APPLICABLE-

      REFERENCES:
9.0
       1. Camarasu CC. Residual solvents determination in the drug products by static head space –
          gas chromatography. Chromatographia supplement 2002; 56: S137- S143.

       2. Puranik SB, Pawar VR, Lalitha N, Sanjay Pai PN and Rao GK. Residual solvent analysis in the
          hydrochloride salts of active ingredients .Pak J Pharm Sci 2009; 22(4):410-414.

       3. Puranik SB, Sanjay Pai PN, Rao GK. Determination of organic volatile impurities in herbal
          formulation and extracts by capillary gas chromatography. International journal of applied
          research in natural products 2009; 2(1): 32-46.
4. Nikolic B, Tesivic B, Dordevic I, Jadranin M, Todosijeuic M, Bojovic S, et al. n- Alkane in
   the needle wax of Pinus heldreichi var.pancic.; J Serb Chem Soc 2010; 75(10): 1337-1346.

5. Uematsu Y, Suzuki K, Iida K, Hirata K, Ueta T and Kamata K. Determination of low levels of
   methanol and ethanol in licorice extract by large volume injection head –space gas
   chromatography. J Food Hyg Soc. japan 2002; 43(5): 295-300.

6. Chun-DI Hu, Liang YZ, Guo, Xiao-Ru LI and Wang WP. Determination of essential oil from
   Osmathus fragans tea by GS- MS combined with a chemometric resolution method.
   Molecules 2010; (15): 3683-3693.

7. Gupta A, Singh Y, Srinivas KS, Jain G, Kumar VB, Semwar VP. Determination and validation
   of a headspace gas chromatographic method for the determination of residual solvents in
   anterolone(RBx11160) maleate bulk drug. J Pharm Bio Sci 2010; 2(1): 32-37.

8.    Sanjay Pai PN, Balaphanisekhar B, Rao GK, Pasha K, Determination of methylene chloride
     organic volatile impurity marketed formulation of ciprofloxacin, norfloxacin, pefloxacin
     and ofloxacin. Ind J Pharm Sci 2007; 69(3): 352-359.

9.    Wadher S J, Puranik M, Yeole PG, Lokhande CS. Determination of ethanol in
     Abhayarishta by gas chromatography. Ind J Pharm Sci 2007; 69(1):152-154.

10. Puranik SB, Sanjay Pai PN, Rao GK. Oraganic volatile impurities in pharmaceutical. Ind J
   Pharm Sci 2007; 69(3):352-358.

11. Karuza JJ, Folvarski K. Validation of the assay method for camphor and menthol in a herbal
    drug preparation. J Pharm Bio Ana 1996; (15): 419-422.

12. Lang YZ, Xie P, Chan k. Quality control of herbal medicines. Journal of Chromatography B
    2004; (812): 53-70.
10    Signature of the candidate:


11.   Remarks of the Guide:            Recommended for Research
12.   Name and Designation of:

      12.1. Institutional Guide:       Dr. MONICA KACHROO
                                       Professor
                                       Department of Pharmaceutical Chemistry,
                                       Al - Ameen College of Pharmacy,
                                       Hosur Road, Bangalore-560 027.
      12.2. Signature:


      12.3. Co-Guide                   Mr. B. Murali
                                       Senior Manager- Analytical chemistry
                                       R&D Center; Natural Remdies:
                                       Plot No. 5B, Veerasandra Indl. Area
                                       19th K. M. Stone, Hosur Road,
                                       Electronic City, Bangalore- 560 100

      12.4. Signature:

      12.5. Head of the Department:    Dr. Gopal Krishna Rao
                                       Professor and Head
                                       Department of Pharmaceutical Chemistry,
                                       Al-Ameen College of Pharmacy,
                                       Hosur Road, Bangalore -560027.


      12.6. Signature


13    13.1. Remarks of the Principal   Forwarded to the University for approval.


      13.2. Signature                  Prof. B. G. Shivananda
                                       Principal
                                       Al-Ameen college of pharmacy
                                       Hosur Road, Bangalore -560 027

								
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