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=
_________________
Average % 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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