SUCRALFATE METHOD OF ANALYSIS SOP

1.0  OBJECTIVE:
To lay down a procedure of analytical report for the active raw material of the Sucralfate from the Pharmacopoeial specifications.
2.0  SCOPE:
This SOP shall be applicable in Q.C laboratory.
3.0  RESPONSIBILITY:
3.1  Q.C Analysts.
4.0  ACCOUNTABILITY:
4.1  Q.C Manager.
5.0  PROCEDURE:
5.1  Characters:
5.1.1        Appearance:
5.1.1.1  White or almost white, amorphous powder.
5.1.2        Solubility:
5.1.2.1  Material and equipment:
5.1.2.1.1        Glassware (4 test tubes, 1 spatula).
5.1.2.1.2        Ethanol (96%).
5.1.2.1.3        Methylene chloride.
5.1.2.1.4        Dilute solutions of mineral acid and alkali hydroxide.
5.1.2.1.5        Purified water.
5.1.2.2  Sample:
5.1.2.2.1        Small quantity.
5.1.2.3  Method:
5.1.2.3.1        Take 4 test tubes and add small quantity of sample for testing solubility according to B.P specifications.
5.1.2.3.2        Add purified water in test tube 1 and observe.
5.1.2.3.3        Add ethanol (96%) in test tube 2 and observe.
5.1.2.3.4        Add Methylene chloride in test tube 3 and observe.
5.1.2.3.5        Add dilute solutions of mineral acid and alkali hydroxide in test tube 4 and observe.
5.1.2.4  Observations:
5.1.2.4.1        The sample in test tube 1, 2 & 3 containing with purified water, ethanol (96%) & Methylene chloride is practically insoluble.
5.1.2.4.2        The sample in test tube 4 containing with dilute solutions of mineral acid and alkali hydroxide is dissolved.
5.2  Identification tests:
5.2.1         
5.2.1.1  Material and equipment:
5.2.1.1.1        Glassware (according to requirement).
5.2.1.1.2        Burner.
5.2.1.1.3        10.0ml of 0.1M hydrochloric acid.
5.2.1.1.4        0.1M sodium hydroxide.
5.2.1.1.5        0.15ml of freshly prepared copper sulphate solution.
5.2.1.1.6        2.0ml of freshly prepared dilute sodium hydroxide.
5.2.1.1.7        4.0ml of dilute hydrochloric acid.
5.2.1.1.8        4.0ml of dilute sodium hydroxide solution.
5.2.1.2  Sample:
5.2.1.2.1        2.0g.
5.2.1.3  Method:
5.2.1.3.1        Take a test tube and add 2.0g of sample in it and add 10.0ml of 0.1M hydrochloric acid and boil it on burner.
5.2.1.3.2        Cool it and neutralize with 0.1M sodium hydroxide.
5.2.1.3.3        Take another test tube add 5.0ml of the above solution.
5.2.1.3.4        Add 0.15ml of freshly prepared copper sulphate solution and 2.0ml of freshly prepared dilute sodium hydroxide.
5.2.1.3.5        The solution is blue and clear.
5.2.1.3.6        Boil on burner the solution remains blue and clear after boiling.
5.2.1.3.7        To the hot solution add 4.0ml of dilute hydrochloric acid and boil for 1 min on burner.
5.2.1.3.8        Add 4.0ml of dilute sodium hydroxide solution.
5.2.1.3.9        Observe the changes.
5.2.1.4  Observations:
5.2.1.4.1        An orange ppt is formed, immediately.
5.2.2        Aluminium test:
5.2.2.1  Material and equipment:
5.2.2.1.1        Glassware (according to requirement).
5.2.2.1.2        Burner.
5.2.2.1.3        0.5ml of dilute hydrochloric acid.
5.2.2.1.4        0.5ml of thioacetamide reagent.
5.2.2.1.5        Dilute sodium hydroxide solution (q.s).
5.2.2.1.6        Ammonium chloride solution (q.s).
5.2.2.1.7        Purified water (q.s).
5.2.2.2  Sample:
5.2.2.2.1        15.0mg.
5.2.2.3  Method:
5.2.2.3.1        Take a test tube and add 15.0mg of sample in it.
5.2.2.3.2        Dissolve it in a mixture of 0.5ml of dilute hydrochloric acid and 2.0ml of purified water.
5.2.2.3.3        Add about 0.5ml of dilute hydrochloric acid and about 0.5ml of thioacetamide reagent.
5.2.2.3.4        No ppt is formed.
5.2.2.3.5        Add drop wise dilute sodium hydroxide solution.
5.2.2.3.6        A gelatinous white ppt is formed.
5.2.2.3.7        Add further dilute sodium hydroxide solution
5.2.2.3.8        Observe the change that gelatinous white ppt is dissolved.
5.2.2.3.9        Gradually add ammonium chloride solution.
5.2.2.3.10    Observe the changes.
5.2.2.4  Observations:
5.2.2.4.1        The gelatinous white ppt is re-formed.
5.3  Assay:
5.3.1        Aluminium:
5.3.1.1  Apparatus:
5.3.1.1.1        Glassware (according to requirement).
5.3.1.1.2        Analytical weighing balance.
5.3.1.1.3        Water bath.
5.3.1.1.4        Magnetic stirrer.
5.3.1.1.5        Titration apparatus.
5.3.1.2  Material and reagents:
5.3.1.2.1        10.0ml of 6M hydrochloric acid.
5.3.1.2.2        10.0ml of 0.1M sodium edetate.
5.3.1.2.3        Ammonium acetate solution.
5.3.1.2.4        Dilute acetic acid.
5.3.1.2.5        25.0ml of ethanol (96%).
5.3.1.2.6        1.0ml of freshly prepared 0.25g/L solution of dithizone in ethanol (96%).
5.3.1.2.7        0.1M zinc sulfate.
5.3.1.2.8        Purified water (q.s).
5.3.1.3  Sample:
5.3.1.3.1        1.0g
5.3.1.4  Method of analysis:
5.3.1.4.1        Sample titration:
5.3.1.4.1.1  Take a beaker of 50.0ml and add 0.1g of sample in it.
5.3.1.4.1.2  Disperse the sample in 10.0ml of 6M hydrochloric acid.
5.3.1.4.1.3  Heat it with continuous stirring in a water bath at 70oC for 5min.
5.3.1.4.1.4  Cool it to room temperature.
5.3.1.4.1.5  Take a 250.0ml of volumetric flask and transfer quantitatively to a volumetric flask and dilute it to 250.0ml with purified water, mix it.
5.3.1.4.1.6  Filter the solution by using filter paper and 1000.0ml of beaker. Discard the 1st portion of the filtrate.
5.3.1.4.1.7  Take a conical flask and add 10.0ml of solution in it.
5.3.1.4.1.8  Add 10.0ml of 0.1M sodium edetate and 30.0ml of mixture of equal volumes of ammonium acetate solution and dilute acetic acid.
5.3.1.4.1.9  Heat it on water bath at 70oC for 5min, and then cool.
5.3.1.4.1.10             Add 25.0ml of ethanol (96%) and 1.0ml of a freshly prepared 0.25g/L solution of dithizone in ethanol (96%).
5.3.1.4.1.11             Set titration apparatus.
5.3.1.4.1.12             Fill titrant 0.1M zinc sulfate in burette.
5.3.1.4.1.13             Titrate the excess of sodium edetate with 0.1M zinc sulfate until the colour changes to pink.
5.3.1.4.1.14             Note down the volume used as shown in Annexure-1.
5.3.1.4.1.15             And take average.
5.3.1.4.2        Blank titration:
5.3.1.4.2.1  Take a beaker of 50.0ml and add 10.0ml of 6M hydrochloric acid.
5.3.1.4.2.2  Heat it with continuous stirring in a water bath at 70oC for 5min.
5.3.1.4.2.3  Cool it to room temperature.
5.3.1.4.2.4  Take a 250.0ml of volumetric flask and transfer quantitatively to a volumetric flask and dilute it to 250.0ml with purified water, mix it.
5.3.1.4.2.5  Filter the solution by using filter paper and 1000.0ml of beaker. Discard the 1st portion of the filtrate.
5.3.1.4.2.6  Take a conical flask and add 10.0ml of solution in it.
5.3.1.4.2.7  Add 10.0ml of 0.1M sodium edetate and 30.0ml of mixture of equal volumes of ammonium acetate solution and dilute acetic acid.
5.3.1.4.2.8  Heat it on water bath at 70oC for 5min, and then cool.
5.3.1.4.2.9  Add 25.0ml of ethanol (96%) and 1.0ml of a freshly prepared 0.25g/L solution of dithizone in ethanol (96%).
5.3.1.4.2.10    Set titration apparatus.
5.3.1.4.2.11    Fill titrant 0.1M zinc sulfate in burette.
5.3.1.4.2.12    Titrate the excess of sodium edetate with 0.1M zinc sulfate until the colour changes to pink.
5.3.1.4.2.13    Note down the volume used as shown in Annexure-1.
5.3.1.4.2.14    And take average.
5.3.1.4.3        Calculate percentage purity.
5.3.1.4.4        Calculations:
5.3.1.4.4.1  After taking average volume of both blank titration and sample titration. Calculate the volume used by the examined substance by using formula:
Volume used by substance = Blank titration - Sample titration.
5.3.1.4.4.2  For percentage purity use formula:
%age purity = volume used by substance x factor x 100
                                                                                Weight of sample
5.3.1.4.4.3  Put values and calculate %age purity.
5.3.1.5  Factor:
5.3.1.5.1        1ml of 0.1M sodium edetate is equivalent to 2.689mg of aluminium Al.
5.3.1.6  Limit:
5.3.1.6.1        16.5% to 18.5%.
6.0  REVISION LOG:
Revision No.
Effective Date
Reason
00

New SOP
7.0  REFERENCES:
7.1  The British Pharmacopoeia. Vol II., Official Monograph / Sucralfate: 2015, pp. 925-926.
8.0  ANNEXURES:
Annexure 1: Assay observations and calculations.
Annexure: 1
Assay observations and calculations (Acid-base titration)
Acid-base titration
Indicator: ___________________
Weight of sample: ____________                                         Factor: 5.832mg.
Titrant: _____________________
Sample titration
Sr.#
Initial volume (vi)
(ml)
Final volume (vf)
(ml)
vf-vi
(ml)
1.



2.



3.



Average volume: _________________
Blank titration
Sr.#
Initial volume (vi)
(ml)
Final volume (vf)
(ml)
vf-vi
(ml)
1.



2.



3.



Average volume: _________________
Calculations:
Volume used by substance = Blank titration - Sample titration.

%age purity = volume used by substance x factor x 100
                                                                     Weight of sample


RESULT: ____________________________________________________________

9.0  ABBREVIATIONS:
Abbreviation
Expanded Form
SOP
Standard operating procedure
&
And
No.
Number  
Ltd.
Limited
Sr.#
Serial number
Q.C
Quality control
%
Percentage
q.s
Quantity sufficient
Ppt
Precipitate
G
Grams
Ml
Milliliter
M
Molar
g/L
Grams per liter
mg
Milligram
oC
Degree centigrade
vi
Initial volume
vf
Final volume
B.P
British pharmacopoeia
Vol
Volume
QCA
Quality control active ingredient
F
Format


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