FERROUS FUMARATE SOP


1.0  OBJECTIVE:
To lay down a procedure for the active raw material of the ferrous fumarate from the Pharmacopoeial specifications.
2.0  SCOPE:
This SOP shall be applicable in Q.C laboratory.
3.0  RESPONSIBILITY:
3.1  Q.C Analyst.
4.0  ACCOUNTABILITY:
4.1  Q.C Manager.
5.0  PROCEDURE:
5.1  Characters:
5.1.1        Appearance:
5.1.1.1  Fine, reddish-orange or reddish-brown powder.
5.1.2        Solubility:
5.1.2.1  Material and equipment:
5.1.2.1.1        Glassware (3 test tubes, 1 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 3 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 purified water is slightly soluble.
5.1.2.4.2        The sample in test tube 2 containing with ethanol (96%) is very slightly soluble.
5.2  Identification tests:
5.2.1         
5.2.1.1  Material and equipment:
5.2.1.1.1        Glassware (1 test tube, 1 pipette).
5.2.1.1.2        Analytical weighing balance.
5.2.1.1.3        1.0g of resorcinol R.
5.2.1.1.4        0.15ml of sulfuric acid R.
5.2.1.1.5        Purified water.
5.2.1.2  Sample:
5.2.1.2.1        0.5g
5.2.1.3  Method:
5.2.1.3.1        Take a test tube and add 0.5g of sample in it.
5.2.1.3.2        Mix it with 1.0g of resorcinol R.
5.2.1.3.3        To 0.5g of the mixture in a crucible add 0.15ml of sulfuric acid R. heat it gently on water bath.
5.2.1.3.4        A dark red semi-solid mass is formed.
5.2.1.3.5        Add the mass, with care to 100.0ml of purified water containing in another beaker.
5.2.1.3.6        Observe the changes.
5.2.1.4  Observations:
5.2.1.4.1        An orange-yellow colour develops and the solution shows no fluorescence.
5.2.2        Iron determination test:
5.2.2.1  Material and equipment:
5.2.2.1.1        Glassware (1 test tube, 1 pipette).
5.2.2.1.2        Analytical weighing balance.
5.2.2.1.3        Water bath.
5.2.2.1.4        Hydrochloric acid.
5.2.2.1.5        Purified water.
5.2.2.2  Sample:
5.2.2.2.1        1.0g.
5.2.2.3  Method:
5.2.2.3.1        Take a test tube and add 1.0g of sample in it.
5.2.2.3.2        Add 25.0ml of a mixture of equal volumes of hydrochloric acid R and purified water R.
5.2.2.3.3        Heat it on water bath for 15 minutes.
5.2.2.3.4        Cool it and filter it by using filtration apparatus.
5.2.2.3.5        Collect the 1.0ml of filtrate in test tube.
5.2.2.3.6        Add 1.0ml of potassium ferricyanide solution R.
5.2.2.3.7        A blue ppt is formed.
5.2.2.3.8        Add 5.0ml of dilute hydrochloric acid R.
5.2.2.3.9        Observe the changes.
5.2.2.4  Observations:
5.2.2.4.1        A blue ppt is formed that does not dissolve on addition of dilute hydrochloric acid.  
5.3  Loss on drying:
5.3.1        Material and equipment:
5.3.1.1  Glassware (according to requirement).
5.3.1.2  Analytical weighing balance.
5.3.1.3  Oven.
5.3.2        Sample:
5.3.2.1  1.000g.
5.3.3        Method:
5.3.3.1  Weigh 1.000g of the test sample.
5.3.3.2  Set the oven apparatus. Operate it according to the SOP.
5.3.3.3  Place the sample into the tray and dry it.
5.3.3.4  Set the temperature of oven at 105oC for 45min.
5.3.3.5  And wait till the sample loses its moisture.
5.3.3.6  After 45min weigh the sample again by using analytical weighing balance i.e. the final weight.
5.3.3.7  Note down readings on given Annexure-1.
5.3.4        Observation:
5.3.4.1  Maximum 1.0%.
5.4  Assay:
5.4.1        Apparatus:
5.4.1.1  Glassware (according to requirement).
5.4.1.2  Titration apparatus.
5.4.1.3  Water-bath.
5.4.2        Material and reagents:
5.4.2.1  7.5ml of dilute sulfuric acid R.
5.4.2.2  25.0ml of purified water.
5.4.2.3  0.1ml of ferroin R.
5.4.2.4  0.1M cerium sulfate.
5.4.3        Sample:
5.4.3.1  0.150g
5.4.4        Method of analysis:
5.4.4.1  Sample titration:
5.4.4.1.1        Take a ground-glass stoppered flask and add 0.150g of sample in it.
5.4.4.1.2        With slight heating on water bath add 7.5ml of dilute sulfuric acid R. Dissolve it.
5.4.4.1.3        Cool it and add 25.0ml of purified water.
5.4.4.1.4        Set titration apparatus.
5.4.4.1.5        Use 0.1ml of ferroin R as indicator.
5.4.4.1.6        Titrate with 0.1M cerium sulfate, until the colour changes from orange to light bluish-green.
5.4.4.1.7        Note down the volume used as shown in Annexure-2.
5.4.4.1.8        And take average.
5.4.4.2  Blank titration:
5.4.4.2.1        Take a ground-glass stoppered flask and add 7.5ml of dilute sulfuric acid R and 25.0ml of purified water.
5.4.4.2.2        Set titration apparatus.
5.4.4.2.3        Use 0.1ml of ferroin R as indicator.
5.4.4.2.4        Titrate with 0.1M cerium sulfate, until the colour changes from orange to light bluish-green.
5.4.4.2.5        Note down the volume used as shown in Annexure-2.
5.4.4.2.6        And take average.
5.4.4.3  Calculate percentage purity.
5.4.4.4  Calculations:
5.4.4.4.1        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.
5.4.4.4.2        For percentage purity use formula:
%age purity = volume used by substance x factor x 100
                                                                                         Weight of sample
5.4.4.4.3        Put values and calculate %age purity.
5.4.5        Factor:
5.4.5.1  1ml of 0.1M cerium sulfate is equivalent to 16.99mg of C4H2FeO4.
5.4.6        Limit:
5.4.6.1  93.0% 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 /Ferrous Fumarate: 2015, pp. 948-950.
7.2  The British Pharmacopoeia. Vol V., Official Monograph /Qualitative Reactions and Tests: 2015, pp. 266-270.
8.0  ANNEXURES:
Annexure 1: Observations of Percentage Loss of drying by using oven.
Annexure 2: Observations and calculations of assay.









Annexure: 1
Observations of percentage loss of drying by using Oven
Percentage loss of drying by using Oven
Weight of Sample = _____________
Time period = _____________
Pressure= _________________
Sr.#
Time (min)
Weight of sample (g)
% Loss of Moisture
Initial weight
Final weight















Average % Loss of Moisture: _____________

% Loss of Moisture:






Remarks: _______________________________________________________________







Annexure: 2
Observations and calculations of assay
Indicator: ___________________
Weight of sample: ____________                                                Factor: ______________
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
%
Percentage
B.P
British pharmacopoeia
ml
Milliliter
oC
Degree centigrade
mg
Milligram
g
Grams
M
Molar
Min
Minutes
h
Hour
Vol
Volume
BM
Biomark
QCA
Quality control active ingredient
F
Format
R
Reagent
vi
Initial volume
vf
Final volume


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