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picture1_Hplc Slideshare 66761 | 12962تحليل الي   كروماتوجرافي 5


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File: Hplc Slideshare 66761 | 12962تحليل الي كروماتوجرافي 5
principles principles a gaseous mobile phase flows under pressure through a heated tube either coated with a liquid stationary phase or packed with liquid stationary phase coated onto a solid ...

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               Principles
               Principles
  A gaseous mobile phase flows under pressure through a heated tube 
    either coated with a liquid stationary phase or packed with liquid 
    stationary phase coated onto a solid support. 
  The analyte is loaded onto the head of the column via a heated injection 
    port where it evaporates. 
  lt then condenses at the head of the column, which is at a lower 
    temperature. 
  The oven temperature is then either held constant or programmed to rise 
    gradually. 
  Once on the column separation of a mixture occurs according to the 
    relative lengths of time spent by its components in the stationary phase. 
  Monitoring of the column effluent can be carried out with a variety of 
    detectors.
              Introduction
              Introduction
  The use of gas chromatography (GC) as a quantitative technique in the 
   analysis of drugs has declined in importance since the advent of HPLC 
   and the increasing sophistication of this technique. 
  However, it does still have a role in certain types of quantitative 
   analysis and has broad application in qualitative analysis. 
  Since HPLC currently dominates quantitative analyses in the 
   pharmaceutical industry, the strengths of GC may be overlooked. 
  Capillary GC is capable of performing much more efficient separations 
   than HPLC although with the limitation that the compounds being 
   analysed must be volatile or must be rendered volatile by formation of 
   a suitable derivative' and must also be thermally stable, 
  GC is widely used in environmental science, brewing, the food 
   industry. perfumery and flavourings analysis, the petrochemical 
   industry, microbiological analyses and clinical biochemistry. 
  Although packed column GC is still used in the pharmaceutical 
   industry, open tubular capillary GC, is the more modern manifestation 
   of GC.
        Applications (طقففف ةءارففق)
    The characterisation of some unformulated drugs, particularly 
     with regard to detection of process impurities.
    Limit tests for solvent residues and other volatile impurities in 
     drug substances
    Sometimes used for quantification of drugs in formulations, 
     particularly if the drug lacks a chromuphore.
    Characterisation of some raw materials used in synthesis of 
     drug molecules.
    Characterisation of volatile oils (which may be used as 
     excipients in formulations), proprietary cough mixtures and 
     tonics. and fatty acids in tixed oils.
    Measurement of drugs and their metabolites in biological fluids.
              Strengths
     Capable of the same quantitative accuracy and precision as 
      high-pressure liquid chromatography (HPLC), particularly 
      when used in conjunction with an internal standard.
     Has much greater separating power than HPLC when used 
      with capillary columns.
     Readily automated.
     Can be used to determine compounds which lack 
      chromophores.
     The mobile phase does not vary and does not require disposal 
      and, even if helium is used as a carrier gas, is cheap 
      compared to the organic solvents used in HPLC.
              Limitations
  
   Only thermally stable and volatile compounds can be 
   analysed.
  
   The sample may require derivatisation to convert it to a 
   volatile form, thus introducing an extra step in analysis 
   and. potentially, interference.
  
   Quantitative sample introduction is more difficult because 
   of the small volumes of sample injected.
  
   Aqueous solutions and salts cannot be injected into the 
   instrument.
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...Principles a gaseous mobile phase flows under pressure through heated tube either coated with liquid stationary or packed onto solid support the analyte is loaded head of column via injection port where it evaporates lt then condenses at which lower temperature oven held constant programmed to rise gradually once on separation mixture occurs according relative lengths time spent by its components in monitoring effluent can be carried out variety detectors introduction use gas chromatography gc as quantitative technique analysis drugs has declined importance since advent hplc and increasing sophistication this however does still have role certain types broad application qualitative currently dominates analyses pharmaceutical industry strengths may overlooked capillary capable performing much more efficient separations than although limitation that compounds being analysed must volatile rendered formation suitable derivative also thermally stable widely used environmental science brewing...

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