FERROUS GLUCONATE SOP


1.0  OBJECTIVE:
To lay down a procedure for the active raw material of the ferrous gluconate 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  Greenish-yellow or grey powder or granules.
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        Hot water.
5.1.2.1.3        Ethanol (96%).
5.1.2.1.4        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 hot purified water in test tube 2 and observe.
5.1.2.3.4        Add ethanol (96%) in test tube 3 and observe.
5.1.2.4  Observations:
5.1.2.4.1        The sample in test tube 1 containing with purified water is freely but slowly soluble and giving a greenish-brown solution.
5.1.2.4.2        The sample in test tube 2 containing with hot purified water is more readily soluble.
5.1.2.4.3        The sample in test tube 3 containing with ethanol (96%) is practically insoluble.
5.2  Solution S:
5.2.1        Material and equipment:
5.2.1.1  Glassware (1 50.0ml of beaker, 1 spatula, 1 glass rod, 1 pipette).
5.2.1.2  Analytical weighing balance.
5.2.1.3  Water bath.
5.2.1.4  Magnetic stirrer.
5.2.1.5  Carbon dioxide free water.
5.2.2        Sample:
5.2.2.1  5.0g.
5.2.3        Preparation of solution S:
5.2.3.1  Take a beaker of 50.0ml and add sample 5.0g of sample in it.
5.2.3.2  Add in it carbon-dioxide free water prepared from distilled water by using pipette.
5.2.3.3  Heat it on water-bath to about 60oC.
5.2.3.4  Allow it to cool.
5.2.3.5  Dilute it to 50.0ml with carbon-dioxide free water R.
5.3  Identification tests:
5.3.1        Iron determination test:
5.3.1.1  Material and equipment:
5.3.1.1.1        Glassware (1 test tube, 1 pipette).
5.3.1.1.2        Analytical weighing balance.
5.3.1.1.3        1.0ml of dilute hydrochloric acid.
5.3.1.1.4        1.0ml of potassium thiocyanate solution R.
5.3.1.1.5        5.0ml of isoamyl alcohol R.
5.3.1.1.6        5.0ml of ether R.
5.3.1.1.7        2.0ml of mercuric chloride solution R.
5.3.1.2  Sample:
5.3.1.2.1        1.0ml of solution S.
5.3.1.3  Method:
5.3.1.3.1        Take a test tube and add 1.0ml of solution S in it.
5.3.1.3.2        Add 1.0ml of dilute hydrochloric acid R and 1.0ml of potassium thiocyanate solution R.
5.3.1.3.3        The solution is coloured red.
5.3.1.3.4        Take two portions, each of 1.0ml, of the mixture. To one portion add 5.0ml of isoamyl alcohol R or 5.0ml of ether R. Shake it and allow it to stand.
5.3.1.3.5        The organic layer is coloured pink.
5.3.1.3.6        To the other portion add 2.0ml of mercuric chloride solution R.
5.3.1.3.7        Observe the changes.
5.3.1.4  Observations:
5.3.1.4.1        The red colour disappears.  
5.4  Loss on drying:
5.4.1        Material and equipment:
5.4.1.1  Glassware (according to requirement).
5.4.1.2  Analytical weighing balance.
5.4.1.3  Oven.
5.4.2        Sample:
5.4.2.1  0.500g.
5.4.3        Method:
5.4.3.1  Weigh 0.500g of the test sample.
5.4.3.2  Set the oven apparatus. Operate it according to the SOP.
5.4.3.3  Place the sample into the tray and dry it.
5.4.3.4  Set the temperature of oven at 105oC for 5h.
5.4.3.5  And wait till the sample loses its moisture.
5.4.3.6  After 5h weigh the sample again by using analytical weighing balance i.e. the final weight.
5.4.3.7  Note down readings on given Annexure-1.
5.4.4        Observation:
5.4.4.1  5.0%-10.5%.
5.5  Assay:
5.5.1        Apparatus:
5.5.1.1  Glassware (according to requirement).
5.5.1.2  Titration apparatus.
5.5.1.3  Water-bath.
5.5.2        Material and reagents:
5.5.2.1  0.5g of sodium hydrogen carbonate R.
5.5.2.2  30.0m of dilute sulfuric acid R.
5.5.2.3  70.0ml of purified water.
5.5.2.4  0.1ml of ferroin R as indicator.
5.5.2.5  0.5M ammonium and cerium nitrate.
5.5.3        Sample:
5.5.3.1  1.0g.
5.5.4        Method of analysis:
5.5.4.1  Sample titration:
5.5.4.1.1        Take a ground-glass stoppered flask and add 0.5g of sodium hydrogen carbonate R in it.
5.5.4.1.2        Add a mixture of 30.0m of dilute sulfuric acid R and 70.0ml of purified water.
5.5.4.1.3        Dissolve it by using magnetic stirrer operate according to SOP.
5.5.4.1.4        When the effervescence stops, dissolve 1.0g of the substance to be examined with gentle shaking.
5.5.4.1.5        Set titration apparatus.
5.5.4.1.6        Use 0.1ml of ferroin R as indicator.
5.5.4.1.7        Titrate with 0.5M ammonium and cerium nitrate.
5.5.4.1.8        Note down the volume used as shown in Annexure-2.
5.5.4.1.9        And take average.
5.5.4.2  Blank titration:
5.5.4.2.1        Take a ground-glass stoppered flask and add 0.5g of sodium hydrogen carbonate R in it.
5.5.4.2.2        Add a mixture of 30.0m of dilute sulfuric acid R and 70.0ml of purified water.
5.5.4.2.3        Dissolve it by using magnetic stirrer operate according to SOP.
5.5.4.2.4        When the effervescence stops, start titration.
5.5.4.2.5        Set titration apparatus.
5.5.4.2.6        Use 0.1ml of ferroin R as indicator.
5.5.4.2.7        Titrate with 0.5M ammonium and cerium nitrate.
5.5.4.2.8        Note down the volume used as shown in Annexure-2.
5.5.4.2.9        And take average.
5.5.4.3  Calculate percentage purity.
5.5.4.4  Calculations:
5.5.4.4.1        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.
5.5.4.4.2        For percentage purity use formula:
%age purity = volume used by substance x factor x 100
                                                                                Weight of sample
5.5.4.4.3        Put values and calculate %age purity.
5.5.5        Factor:
5.5.5.1  1ml of 0.1M ammonium and cerium nitrate is equivalent to 5.585mg of iron (II).
5.5.6        Limit:
5.5.6.1  11.8% to 12.5% of iron (II).
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 Gluconate: 2015, pp. 950-951.
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
RM
Raw Material 
QCA
Quality control active ingredient
F
Format
R
Reagent
vi
Initial volume
vf
Final volume


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