ASPIRIN SOP


ASPIRIN SOP

1.0  OBJECTIVE:
To lay down a procedure for the active raw material of the Aspirin (Acetylsalicylic acid) 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 powder.
5.1.1.2  Crystalline powder.
5.1.1.3  Colourless.
5.1.2        Solubility:
5.1.2.1  Material and equipment:
5.1.2.1.1        Glassware (test tubes, spatula).
5.1.2.1.2        Ethanol (96%).
5.1.2.1.3        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 2 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.
5.1.2.4  Observations:
5.1.2.4.1        The sample in test tube 1 containing with water is slightly soluble.
5.1.2.4.2        The sample in test tube 2 containing with ethanol (96%) is freely soluble.
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        Melting point apparatus (beaker, stirrer, thermometer, capillary tube, burner, thread).
5.2.1.1.3        Desiccator.
5.2.1.1.4        Dilute sodium hydroxide.
5.2.1.1.5        Dilute sulfuric acid.
5.2.1.1.6        Purified water.
5.2.1.2  Sample:
5.2.1.2.1        0.2g.
5.2.1.3  Method:
5.2.1.3.1        Take a 50.0ml of beaker and add 0.2g of sample in it.
5.2.1.3.2        Add 4ml of dilute sodium hydroxide solution in it with the help of pipette.
5.2.1.3.3        Boil it for 3min.
5.2.1.3.4        Cool it.
5.2.1.3.5        Add 5.0ml of dilute sulfuric acid with the help of pipette.
5.2.1.3.6        A crystalline ppt formed.
5.2.1.3.7        Filter it.
5.2.1.3.8        Wash the ppt with the help of water.
5.2.1.3.9        Dry at 100-105oC in desiccator.
5.2.1.3.10    And then find out the melting point of the ppt by using melting point apparatus.
5.2.1.3.11    Melting point determination method:
5.2.1.3.11.1    Firstly set the apparatus.
5.2.1.3.11.2          Fill 100ml beaker with water and place wire gauze on tripod stand, put beaker on it.
5.2.1.3.11.3          Heat up the capillary tube on burner from center such that it divides into two upon pulling the capillary tube from both sides in opposite directions.
5.2.1.3.11.4          Introduce a sufficient quantity into a capillary tube to give a compact column 4mm to 6mm in height.
5.2.1.3.11.5          Tie up the capillary tube near the thermometer bulb with the help of thread.
5.2.1.3.11.6          And hang the thermometer on stand such that the capillary tube is not fully immersed in water. The immersion mark of which is at the level of the surface of the liquid.
5.2.1.3.11.7          Allow the burner to heat up the liquid in beaker.
5.2.1.3.11.8          Observe it closely.
5.2.1.3.11.9          Record the temperature at which the last particle passes into the liquid phase.
5.2.1.4  Observations:
5.2.1.4.1        The melting point is 156oC-161oC.
5.2.2         
5.2.2.1  Material and equipment:
5.2.2.1.1        Glassware (according to requirement).
5.2.2.1.2        Calcium hydroxide.
5.2.2.1.3        Nitrobenzaldehyde solution.
5.2.2.1.4        Dilute hydrochloric acid.
5.2.2.1.5        Filter paper.
5.2.2.1.6        Purified water.
5.2.2.2  Sample:
5.2.2.2.1        0.1g.
5.2.2.3  Method:
5.2.2.3.1        Take a test tube and mix 0.1g of substance to be examined with 0.5g of calcium hydroxide.
5.2.2.3.2        Heat the mixture on water bath.
5.2.2.3.3        Expose it to the fumes produced a piece of filter paper impregnated with 0.05ml of nitrobenzyaldehyde solution.
5.2.2.3.4        Observe the changes.
5.2.2.3.5        Take a filter paper and moisten with the dilute hydrochloric acid.
5.2.2.3.6        Observe the changes.
5.2.2.4  Observations:
5.2.2.4.1        A greenish-blue or greenish-yellow colour develops on the filter paper impregnated with nitrobenzyaldehyde.
5.2.2.4.2        The moisten filter paper with dilute hydrochloric acid colour become blue.
5.2.3        Salicylates test:
5.2.3.1  Material and equipment:
5.2.3.1.1        Glassware (according to requirement).
5.2.3.1.2        0.5ml of ferric chloride.
5.2.3.1.3        0.1ml of acetic acid.
5.2.3.1.4        Purified water.
5.2.3.2  Sample:
5.2.3.2.1        20.0mg.
5.2.3.3  Method of analysis:
5.2.3.3.1        Take a test tube and take in it 20.0mg of the ppt obtained in identification test 5.2.1.
5.2.3.3.2        Add 10.0ml of water in it and dissolve it upon heating.
5.2.3.3.3        Cool it.
5.2.3.3.4        And then take 1.0ml of the above solution in another test tube for identification of salicylates.
5.2.3.3.5        Add 0.5ml of ferric chloride solution.
5.2.3.3.6        Observe the colour change.
5.2.3.3.7        And after that add 0.1ml of acetic acid.
5.2.3.3.8        Observe again.
5.2.3.4  Observations:
5.2.3.4.1        A violet colour is produced upon addition of ferric chloride.
5.2.3.4.2        That violet colour persists after the addition of acetic acid.
5.3  Assay:
5.3.1        Apparatus:
5.3.1.1  Glassware (according to requirement).
5.3.1.2  Titration apparatus.
5.3.1.3  Water-bath.
5.3.2        Material and reagents:
5.3.2.1  Alcohol.
5.3.2.2  0.5M alcoholic potassium hydroxide.
5.3.2.3  Dilute nitric acid.
5.3.2.4  0.1M silver nitrate.
5.3.2.5  Ferric ammonium sulphate solution.
5.3.2.6  0.1M ammonium thiocyanate.
5.3.2.7  Purified water.
5.3.3        Sample:
5.3.3.1  0.2g.
5.3.4        Method of analysis:
5.3.4.1  Sample titration:
5.3.4.1.1        Take a ground-glass stoppered flask and take in it 1.0g of sample.
5.3.4.1.2        Dissolve it in 10.0ml of ethanol (96%).
5.3.4.1.3        Add 50.0ml of 0.5M sodium hydroxide.
5.3.4.1.4        Close the flask and allow it to stand for 1h.
5.3.4.1.5        Set titration apparatus.
5.3.4.1.6        Use 0.2ml of phenolphthalein solution as indicator.
5.3.4.1.7        Titrate with 0.5M hydrochloric acid.
5.3.4.1.8        Note down the volume used as shown in Annexure-1.
5.3.4.1.9        And take average.
5.3.4.2  Blank titration:
5.3.4.2.1        Take a ground-glass stoppered flask and add 10.0ml of ethanol (96%).
5.3.4.2.2        And add 50.0ml of 0.5M sodium hydroxide and dissolve it.
5.3.4.2.3        Close the flask and allow it to stand for 1h.
5.3.4.2.4        Set titration apparatus.
5.3.4.2.5        Use 0.2ml of phenolphthalein solution as indicator.
5.3.4.2.6        Titrate with 0.5M hydrochloric acid.
5.3.4.2.7        Note down the volume used as shown in Annexure-1.
5.3.4.2.8        And take average.
5.3.4.3  Calculate percentage purity.
5.3.4.4  Calculations:
5.3.4.4.1        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.
5.3.4.4.2        For percentage purity use formula:
%age purity = volume used by substance x factor x 100
                                                                                         Weight of sample
5.3.4.4.3        Put values and calculate %age purity.
5.3.5        Factor:
5.3.5.1  1ml of 0.5M Sodium hydroxide is equivalent to 45.04mg of C9H8O4.
5.3.6        Limit:
5.3.6.1  99.5% to 101.0% (dried substance).
6.0  REVISION LOG:
Revision No.
Effective Date
Reason
00

New SOP

7.0  REFERENCES:
7.1  The British Pharmacopoeia. Vol I., Official Monograph /Aspirin: 2015, pp. 204-205.
8.0  ANNEXURES:
Annexure 1: Observations and calculations.


Annexure: 1
Observations and calculations
Indicator: ___________________
Weight of sample: ____________                                                Factor: ____45.04mg.__
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
B.P
British pharmacopoeia
g
Grams
ml
Milliliter
Min
Minutes
ppt
Precipitates
oC
Degree centigrade
mm
Millimeter
mg
Milligram
M
Molar
h
Hour
Vol
Volume
vi
Initial volume
vf
Final volume
QCA
Quality control active ingredient
F
Format


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