OMEPRAZOLE SODIUM SOP
1.0 OBJECTIVE:
To
lay down a procedure for the active raw material of the Omeprazole sodium 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
Hygroscopic
powder.
5.1.2
Solubility:
5.1.2.1
Material and equipment:
5.1.2.1.1
Glassware (4 test
tubes, 1 spatula).
5.1.2.1.2
Ethanol (96%).
5.1.2.1.3
Purified water.
5.1.2.1.4
Propylene glycol.
5.1.2.1.5
Methylene
chloride.
5.1.2.2
Sample:
5.1.2.2.1
Small quantity.
5.1.2.3
Method:
5.1.2.3.1
Take 4 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
5.1.2.3.4
Add Propylene
glycol in test tube 3 and observe.
5.1.2.3.5
Add Methylene
chloride in test tube 4 and observe.
5.1.2.4
Observations:
5.1.2.4.1
The sample in test
tube 1 & 2 containing with purified water and Ethanol (96%) is freely soluble.
5.1.2.4.2
The sample in test
tube 3 containing with Propylene glycol is soluble.
5.1.2.4.3
The sample in test
tube 4 containing with Methylene chloride is very 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
0.50g.
5.2.3
Preparation of solution
S:
5.2.3.1
Take a beaker of
50.0ml and add sample 0.50g in it.
5.2.3.2
Add in it sufficient
quantity of Carbon dioxide free water and mix by using magnetic stirrer i.e.
SOP
5.2.3.3
Dilute it to
25.0ml with the same solvent.
5.3 Identification
tests:
5.3.1
Optical
rotation:
5.3.1.1
Material and equipment:
5.3.1.1.1
Polarimeter.
5.3.1.1.2
Analytical weighing
balance.
5.3.1.1.3
Magnetic stirrer.
5.3.1.1.4
Glassware (1
beaker of 50.0ml, 1 stirrer, 1 spatula).
5.3.1.1.5
Purified water.
5.3.1.2
Sample:
5.3.1.2.1
Solution S.
5.3.1.3
Method:
5.3.1.3.1
Take a beaker of
50.0ml and add Solution S in it.
5.3.1.3.2
Firstly clean the
Polarimeter with clean dry cloth, according to SOP.
5.3.1.3.3
Operate the
Polarimeter according to SOP.
5.3.1.3.4
Fill the
Polarimeter tube with blank solution and determine the observed optical
rotation.
5.3.1.3.5
Similarly, fill
the Polarimeter tube with sample solution and determine the observed optical
rotation.
5.3.1.3.6
Note down the
values in annexure-1.
5.3.1.4
Observations:
5.3.1.4.1
-0.10o
to +0.10o.
5.3.2
Determination
of sodium salts:
5.3.2.1
Material and equipment:
5.3.2.1.1
Glassware (according
to requirement).
5.3.2.1.2
Analytical
weighing balance.
5.3.2.1.3
Burner.
5.3.2.1.4
Ice-water.
5.3.2.1.5
1.5ml of
methoxyphenylacetic reagent R.
5.3.2.1.6
1.0ml of dilute
ammonia R1.
5.3.2.1.7
1.0ml of ammonium
carbonate solution R.
5.3.2.1.8
Purified water
5.3.2.2
Sample:
5.3.2.2.1
1.0g of sample.
5.3.2.3
Method:
5.3.2.3.1
Ignite 1.0g of
sample in a china dish. And cool it.
5.3.2.3.2
Add 1.0ml of purified
water to the above obtained residue.
5.3.2.3.3
Neutralize it with
hydrochloric acid.
5.3.2.3.4
Filter it by using
filtration apparatus.
5.3.2.3.5
The obtained
filtrate is diluted to 4.0ml with purified water.
5.3.2.3.6
Take 0.1ml of the
above solution.
5.3.2.3.7
Add 1.5ml of
methoxyphenylacetic reagent R.
5.3.2.3.8
Cool in ice-water
for 30min.
5.3.2.3.9
Observe the
changes.
5.3.2.3.10 A
voluminous, white, crystalline ppt is formed.
5.3.2.3.11 Place
in water at 20oC and stir for 5min.
5.3.2.3.12 The
ppt does not disappear.
5.3.2.3.13 Add
1.0ml of dilute ammonia R1.
5.3.2.3.14 The
ppt dissolves completely.
5.3.2.3.15 Add
1.0ml of ammonium carbonate solution R.
5.3.2.3.16 Observe
the changes.
5.3.2.4
Observations:
5.3.2.4.1
No 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
50.0ml of purified
water.
5.4.2.2
0.1M hydrochloric
acid.
5.4.3
Sample:
5.4.3.1
0.300g.
5.4.4
Method
of analysis:
5.4.4.1 Take
a 100.0ml of beaker and take 0.300g of sample in it.
5.4.4.2 Add
50.0ml of purified water in it dissolve it by using magnetic stirrer i.e..
5.4.4.3 Fill
the right hand side burette with titrant 0.1M hydrochloric acid.
5.4.4.4 Carry
out a Potentiometric titration.
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-2.
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-2.
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 hydrochloric acid corresponds to 36.74mg of Omeprazole sodium C17H18N3NaO3S.
5.4.6
Limit:
5.4.6.1 98.0%
to 101.0% (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 / Omeprazole: 2015, pp. 442-444.
8.0 ANNEXURES:
Annexure 1: Optical
rotation observations and calculations
Annexure 2: Assay
observations and calculations (Potentiometric titration).
Annexure:
1
Optical
rotation observations and calculations
|
Optical
rotation
Instrument:
___________________
Date: _______________
Model:
_______________________ Length
of Polarimeter tube: ________________
Sample:
________________________________g.
Solvent:
________________________________ml.
Concentration
of sample solution: ____________g/ml.
Blank solution:
Average: _______________
Optical
rotation of blank solution: _______________
Sample solution:
Average: _______________
Optical
rotation of sample solution: ______________
Optical rotation of substance = Blank solution - Sample
solution.
Specific
optical rotation of sample solution by using formula:
[α]λ T = α/lc
Result: ________________
Remarks:
___________________________________________________________
|
Annexure:
2
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
|
|
v/s
|
Verses
|
|
mV
|
Millivolts
|
|
g
|
Grams
|
|
ml
|
Milliliter
|
|
Min
|
Minutes
|
|
oC
|
Degree
centigrade
|
|
mg
|
Milligram
|
|
M
|
Molar
|
|
%
|
Percentage
|
|
R
|
Reagent
|
|
o
|
Degree
(angle)
|
|
l
|
Length
|
|
g
|
Grams
|
|
c
|
Concentration
(g/ml)
|
|
g/ml
|
Gram
per milliliter
|
|
α
|
Alpha
|
|
λ
|
Lambda
|
|
T
|
Temperature
|