SODIUM PICOSULFATE METHOD OF ANALYSIS SOP
1.0 OBJECTIVE:
To
lay down a procedure for the active raw material of the Sodium Picosulfate 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
White or almost
white.
5.1.1.2
Crystalline
powder.
5.1.2
Solubility:
5.1.2.1
Material and equipment:
5.1.2.1.1
Glassware (2 test
tubes, 1 spatula, 1 pipette).
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 a test tube
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 1 and observe.
5.1.2.4
Observations:
5.1.2.4.1
The sample in test
tube 1 containing with purified water is freely soluble.
5.1.2.4.2
The sample in test
tube 1 containing with Ethanol (96) is slightly soluble.
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
Magnetic stirrer.
5.2.1.4
Carbon-dioxide
free water.
5.2.2
Sample:
5.2.2.1
2.5g.
5.2.3
Preparation of solution
S:
5.2.3.1
Take a beaker of
50.0ml and add sample 2.5g in it.
5.2.3.2
Add in it
sufficient quantity of carbon-dioxide free water prepared from distilled water.
5.2.3.3
Dilute it to 50.0ml
with the same solvent.
5.3 Identification
tests:
5.3.1
5.3.1.1
Material and equipment:
5.3.1.1.1
Glassware (1 test
tube, 1 spatula, 1 pipette).
5.3.1.1.2
Burner.
5.3.1.1.3
1.0ml of dilute
hydrochloric acid.
5.3.1.1.4
1.0ml of barium
chloride solution.
5.3.1.2
Sample:
5.3.1.2.1
5.0ml of solution
S.
5.3.1.3
Method:
5.3.1.3.1
Take a beaker and
add 5.0ml of solution S in it.
5.3.1.3.2
And add 1.0ml of
dilute hydrochloric acid.
5.3.1.3.3
Heat it on burner
till boiling.
5.3.1.3.4
Add 1.0ml of
barium chloride solution.
5.3.1.3.5
Observe the
changes.
5.3.1.4
Observations:
5.3.1.4.1
A white ppt is
formed.
5.3.2
5.3.2.1
Material and equipment:
5.3.2.1.1
Glassware (1 test
tube, 1 spatula, 1 pipette).
5.3.2.1.2
Analytical
weighing balance.
5.3.2.1.3
3.0ml of sulfuric
acid.
5.3.2.1.4
0.1ml of potassium
dichromate solution R1.
5.3.2.2
Sample:
5.3.2.2.1
10.0mg.
5.3.2.3
Method:
5.3.2.3.1
Take a test tube
and add in it 10.0mg of sample.
5.3.2.3.2
Add 3.0ml of
sulfuric acid and 0.1ml of potassium dichromate solution R1
5.3.2.3.3
Observe the
changes.
5.3.2.4
Observations:
5.3.2.4.1
A violet colour
develops.
5.3.3
Sodium
test:
5.3.3.1
Material and equipment:
5.3.3.1.1
Glassware (test
tube, spatula, beaker, glass rod).
5.3.3.1.2
Analytical
weighing balance.
5.3.3.1.3
Burner.
5.3.3.1.4
2.0ml of 150g/L
solution of potassium carbonate.
5.3.3.1.5
4.0ml of potassium
pyroantimonate solution.
5.3.3.1.6
Iced water.
5.3.3.1.7
Purified water.
5.3.3.2
Sample:
5.3.3.2.1
2.0ml of solution
S.
5.3.3.3
Method:
5.3.3.3.1
Take a test tube
and add 2.0ml of solution S.
5.3.3.3.2
Add 2.0ml of
150g/L solution of potassium carbonate and heat it to boiling on burner.
5.3.3.3.3
Observe the
changes.
5.3.3.3.4
No ppt is formed.
5.3.3.3.5
Add 4.0ml of
potassium pyroantimonate solution again heat it to boiling on burner.
5.3.3.3.6
And then take a
beaker of filled with iced water, put test tube in it and allow it to cool.
5.3.3.3.7
If necessary rub
the inside of the test tube with a glass rod.
5.3.3.3.8
Observe the
changes.
5.3.3.4
Observations:
5.3.3.4.1
A dense white ppt
is formed.
5.4 Assay:
5.4.1
Apparatus:
5.4.1.1
Glassware
(according to requirement).
5.4.1.2
Potentiometer.
5.4.1.3
Magnetic stirrer.
5.4.2
Material
and reagents:
5.4.2.1
80.0ml of
methanol.
5.4.2.2
0.1M Perchloric
acid.
5.4.2.3
Crystal violet
solution.
5.4.3
Sample:
5.4.3.1
0.4g.
5.4.4
Method
of analysis:
5.4.4.1 Take
a 100.0ml of beaker and take 0.4g of sample in it.
5.4.4.2 Add
80.0ml of methanol in it and dissolve by using magnetic stirrer i.e. SOP
5.4.4.3 Fill
the right hand side burette with titrant 0.1M Perchloric acid.
5.4.4.4 Carry
out a Potentiometric titration using crystal violet solution as an indicator.
5.4.4.5 Operate
potentiometer according to SOP
5.4.4.6 To
neutralize analyte add titrant fixed volume (1ml, 0.5ml or 0.1ml) from burette
every time note the reading of change in potential difference (millivolts) for
each addition in given annexure-1.
5.4.4.7 Plot
a graph, volume used v/s millivolts.
5.4.4.8 Find
out the END POINT.
5.4.4.9 Peak
of graph indicates END POINT i.e. the point at which maximum millivolts. Note
down volume used at that point.
5.4.4.10 Perform
blank titration without using sample. Similarly, as sample titration performed.
Record observations in annexure-1.
5.4.4.11 Calculate
volume used by substance by using formula:
Volume
used by substance = Blank titration - Sample titration.
5.4.4.12 Calculate
percentage purity of the sample by using formula:
%age
purity = volume used by substance x factor x 100
Weight of sample
5.4.5
Factor:
5.4.5.1 1ml
of 0.1M Perchloric acid is equivalent to 48.14mg of Sodium Picosulfate C18H13NNa2O8S2.
5.4.6
Limit:
5.4.6.1
98.5% to 100.5%
(anhydrous substance).
6.0 REVISION LOG:
|
Revision No.
|
Effective Date
|
Reason
|
|
00
|
|
New SOP
|
7.0 REFERENCES:
7.1
The British
Pharmacopoeia. Vol II.,
Official Monograph / Sodium
Picosulfate: 2015, pp. 860-861.
7.2
The British
Pharmacopoeia. Vol V.,
Official Monograph /Qualitative Reactions and Tests: 2015, pp. 266-270.
8.0 ANNEXURES:
Annexure 1: Assay
observations and calculations (Potentiometric titration).
Annexure:
1
Assay
observations and calculations (Potentiometric titration)
|
Potentiometric titration
Reference
electrode: ___________________
Indicator
electrode: ____________________
Speed
of magnetic stirrer: _______________
Titrant
used: __________________________
Indicator:
____________________________
Blank
titration:
Plot a graph, volume used v/s millivolts and find out peak
of graph i.e. END POINT of blank titration.
Sample
titration:
Plot a graph, volume used v/s millivolts and find out peak
of graph i.e. END POINT of sample titration:
Volume used by Blank titration: __________________
Volume used by Sample titration: _________________
Volume used by substance = Blank titration - Sample
titration.
mV used by Blank titration: __________________
mV used by Sample titration: _________________
mV used by substance = Blank
titration - Sample titration.
Volume
used by substance: _______________________
Voltmeter
(mV) used by substance: _________________
RESULT: ____________________________________________________________
|
9.0 ABBREVIATIONS:
|
Abbreviation
|
Expanded Form
|
|
SOP
|
Standard
operating procedure
|
|
&
|
And
|
|
No.
|
Number
|
|
Ltd.
|
Limited
|
|
QCA
|
Quality
control active ingredient
|
|
F
|
Format
|
|
Q.C
|
Quality
control
|
|
Vol
|
Volume
|
|
mg
|
Milligram
|
|
ml
|
Milliliter
|
|
ppt
|
Precipitate
|
|
M
|
Molar
|
|
g
|
Grams
|
|
%
|
Percentage
|
|
v/s
|
Verses
|
|
mV
|
Millivolts
|
|
R
|
Reagent
|
|
BP
|
British
Pharmacopoeia
|