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    Assay

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    jaimurugesh

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    © All Rights Reserved
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    Assay

    Uploaded by

    jaimurugesh
    16 views3 pages

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    © All Rights Reserved
    Download as DOCX, PDF, TXT or read online from Scribd
    Download as docx, pdf, or txt
    16 views3 pages

    Assay

    Uploaded by

    jaimurugesh

    Copyright:

    © All Rights Reserved
    Download as DOCX, PDF, TXT or read online from Scribd
    Download as docx, pdf, or txt
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    Assay—

    Mobile phase— Dissolve 132 g of ammonium sulfate in 900 mL of water, dilute

    with water to 1000 mL, and mix. Adjust with phosphoric acid to a pH of 3.5 ± 0.1,

    filter, and degas. Make adjustments if necessary 

    Standard preparation— Dissolve an accurately weighed quantity of sucralfate

    working standard in Mobile phase, and dilute quantitatively, and stepwise if

    necessary, with Mobile phase to obtain a solution having a known concentration

    of about 10 mg of anhydrous potassium sucrose octasulfate (as determined from

    the concentration of USP Potassium Sucrose Octasulfate RS corrected for water

    content by a titrimetric water determination) per mL.

    Assay preparation— Transfer about 450 mg of Sucralfate equivalent cream

    accurately weighed, to a 35-mL centrifuge tube, and shake at a moderate rate on

    a vortex mixer. While shaking add 10.0 mL of a mixture of 4.0 N sulfuric acid and

    2.2 N sodium hydroxide (1:1). Sonicate with swirling for 5 minutes, keeping the

    temperature of the mixture below 30°. Without delay transfer the tube to a vortex

    mixer and while shaking at moderate rate, add an accurately measured volume, V,

    in mL, of 0.1 N sodium hydroxide to bring the pH of the solution to approximately

    2, and dilute the solution with (15.0 − V) mL of water. Shake for 1 minute, and

    centrifuge for 5 minutes. Separate the clear supernatant layer, and allow it to
    stand at room temperature until the pH stabilizes. If the pH is not between 2.3 and

    3.5, repeat the test using a different volume of 0.1 N sodium hydroxide. Use the

    clear supernatant layer.

    The liquid chromatograph is equipped with a refractive index detector and a 3.9-

    mm × 30-cm column that contains packing L8. The detector and column

    temperatures are maintained at 30°. The flow rate is about 1 mL per minute.

    Chromatograph the Standard preparation, and record the peak responses as

    directed for Procedure: the column efficiency determined from the sucrose

    octasulfate peak is not less than 400 theoretical plates; the tailing factor for the

    sucrose octasulfate peak is not more than 4.0; and the relative standard deviation

    for replicate injections is not more than 2.0%.

    Procedure— Separately inject equal volumes (about 50 µL) of the Standard

    preparation and the Assay preparation into the chromatograph, record the

    chromatograms, and measure the responses for the major peaks.

    Content of sucralfate in 50 ml of sample:

    Sample area     std wt        25        wt/ml     %sucrose octa sulfate in std          100     50

    ----------------X---------X--------X----------X---------------------------- ----X-----X

    Std area             25       sam.wt                          100                                34

    Where 34 is corresponding to 100 % of sucralfate.


    Reference sucralfate tablets IP

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