OMEPRAZOLE
SOP
1.0 OBJECTIVE:
To
lay down a procedure for the active raw material of the Omeprazole 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 powder.
5.1.2
Solubility:
5.1.2.1
Material and equipment:
5.1.2.1.1
Glassware (5 test
tubes, 1 spatula).
5.1.2.1.2
Ethanol (96%).
5.1.2.1.3
Purified water.
5.1.2.1.4
Methanol.
5.1.2.1.5
Dilute solutions
of alkali hydroxides (e.g. dil. NaOH).
5.1.2.1.6
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 5 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 Methylene
chloride in test tube 2 and observe
5.1.2.3.4
Add Ethanol (96%)
in test tube 3 and observe.
5.1.2.3.5
Add Methanol in
test tube 4 and observe.
5.1.2.3.6
Add dil. NaOH in
test tube 5 and observe
5.1.2.4
Observations:
5.1.2.4.1
The sample in test
tube 1 containing with purified water is very slightly soluble.
5.1.2.4.2
The sample in test
tube 2 containing with Methylene chloride is soluble.
5.1.2.4.3
The sample in test
tube 3 & 4 containing with Ethanol (96%) and methanol is sparingly soluble.
5.1.2.4.4
The sample in test
tube 5 containing with dil. NaOH is dissolve.
5.2 Loss
on drying:
5.2.1
Material and equipment:
5.2.1.1
Glassware
(according to requirement).
5.2.1.2
Desiccator.
5.2.1.3
Diphosphorous
pentaoxide (desiccant).
5.2.1.4
Analytical
weighing balance.
5.2.1.5
Spatula.
5.2.2
Sample:
5.2.2.1
1.0g.
5.2.3
Method:
5.2.3.1
Weigh 1g of the
test sample.
5.2.3.2
Set the desiccator
apparatus with desiccant.
5.2.3.3
Operate the desiccator
according to the SOP.
5.2.3.4
Place the sample
into the china dish or petri dish.
5.2.3.5
Set the
temperature 60oC and at 0.1kPa pressure for at least 4h.
5.2.3.6
And wait till the
sample loses its moisture.
5.2.3.7
After 4h weigh the
sample again by using analytical weighing balance i.e. the final weight.
5.2.3.8
Note down readings
on given Annexure-1.
5.2.4
Observations:
5.2.4.1
Maximum 0.5%.
5.3 Assay:
5.3.1
Apparatus:
5.3.1.1
Glassware
(according to requirement).
5.3.1.2
Potentiometer.
5.3.1.3
Magnetic stirrer.
5.3.2
Material
and reagents:
5.3.2.1
10.0ml of purified
water.
5.3.2.2
40.0ml of ethanol
(96%).
5.3.2.3
0.1M sodium
hydroxide.
5.3.2.4
Thymolphthalein
solution (as indicator).
5.3.3
Sample:
5.3.3.1
0.250g.
5.3.4
Method
of analysis:
5.3.4.1 Take
a 100.0ml of beaker and take 0.250g of sample in it.
5.3.4.2 Add
a mixture of 10.0ml of purified water and 40.0ml of ethanol (96%) dissolve by
using magnetic stirrer.
5.3.4.3 Fill
the right hand side burette with titrant 0.1M sodium hydroxide.
5.3.4.4 Carry
out a Potentiometric titration using thymolphthalein solution (as indicator).
5.3.4.5 Operate
potentiometer according to SOP.
5.3.4.6 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.
5.3.4.7 Plot
a graph, volume used v/s millivolts.
5.3.4.8 Find
out the END POINT.
5.3.4.9 Peak
of graph indicates END POINT i.e. the point at which maximum millivolts. Note
down volume used at that point.
5.3.4.10 Perform
blank titration without using sample. Similarly, as sample titration performed.
Record observations in annexure-2.
5.3.4.11 Calculate
volume used by substance by using formula:
Volume used by substance = Blank
titration - Sample titration.
5.3.4.12 Calculate
percentage purity of the sample by using formula:
%age purity = volume used by
substance x factor x 100
Weight
of sample
5.3.5
Factor:
5.3.5.1 1ml
of 0.1M sodium hydroxide is equivalent to 34.54mg of Omeprazole C17H19N3O3S.
5.3.6
Limit:
5.3.6.1 99.0%
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 II.,
Official Monograph / Omeprazole: 2015, pp. 439-441.
8.0 ANNEXURES:
Annexure 1: Observations
of Percentage Loss of drying by using oven.
Annexure 2: Assay
observations and calculations (Potentiometric titration).
Annexure: 1
Observations
of percentage loss of drying
|
Percentage
loss of drying
Apparatus:
____________________
Temperature:
__________________
Pressure:
_____________________
Weight
of Sample = _____________
Time
period = _____________
Average % Loss of Moisture: _____________
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
|