VENLAFAXINE HYDROCHLORIDE METHOD OF ANALYSIS SOP
1.0 OBJECTIVE:
To
lay down a procedure for the active raw material of the Venlafaxine hydrochloride 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 (2 test
tubes, 1 spatula).
5.1.2.1.2
Methanol.
5.1.2.1.3
Anhydrous ethanol.
5.1.2.1.4
Purified water.
5.1.2.1.5
Acetone.
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 methanol in
test tube 2 and observe.
5.1.2.3.4
Add anhydrous
ethanol in test tube 3 and observe.
5.1.2.3.5
Add acetone in
test tube 4 and observe.
5.1.2.4
Observations:
5.1.2.4.1
The sample in test
tube 1and 2 containing with purified water and methanol is freely soluble,
respectively.
5.1.2.4.2
The sample in test
tube 3 containing with anhydrous ethanol is soluble.
5.1.2.4.3
The sample in test
tube 4 containing with acetone is slightly soluble or practically insoluble.
5.2 Identification
tests:
5.2.1
Chlorides
test:
5.2.1.1
Material and equipment:
5.2.1.1.1
Glassware
(according to requirement).
5.2.1.1.2
Centrifuge
machine.
5.2.1.1.3
Dilute nitric
acid.
5.2.1.1.4
Purified water
(q.s).
5.2.1.1.5
0.4ml of Silver
nitrate R1.
5.2.1.1.6
1.5ml of ammonia.
5.2.1.2
Sample:
5.2.1.2.1
Quantity of
substance to be examined equivalent to about 2.0mg of chloride.
5.2.1.3
Method:
5.2.1.3.1
Take a test tube
add in it 2.0ml of water with the help of pipette.
5.2.1.3.2
Dissolve in 2.0ml
of water a quantity of the substance to be equivalent to about 2.0mg of
chloride.
5.2.1.3.3
Acidify with
dilute nitric acid.
5.2.1.3.4
And add 0.4ml of
silver nitrate R1.
5.2.1.3.5
Shake and allow it
to stand.
5.2.1.3.6
A curdled, white
ppt is formed.
5.2.1.3.7
Centrifuge it in
centrifugation machine, according to SOP.
5.2.1.3.8
The obtained ppt
is wash with 3 quantities, each of 1ml, of water.
5.2.1.3.9
Carry out this
operation rapidly is subdued light, degrading the fact that the supernatant
solution may not become perfectly clear.
5.2.1.3.10 Suspend
the precipitate in 2.0ml of water and add 1.5ml of ammonia.
5.2.1.4
Observations:
5.2.1.4.1
The precipitate
dissolves easily with the possible exception of a few large particles which dissolves
slowly.
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
Desiccator.
5.3.2
Sample:
5.3.2.1
1.0g.
5.3.3
Method:
5.3.3.1
Weigh 1.0g of the
test sample.
5.3.3.2
Set the desiccator
apparatus with desiccant (Diphosphorous pentaoxide)
5.3.3.3
Operate the
desiccator according to the SOP.
5.3.3.4
Place the sample
into the china dish or petri dish and dry it.
5.3.3.5
Set the
temperature 80oC and vacuum for at least 3hours.
5.3.3.6
And wait till the
sample loses its moisture.
5.3.3.7
After 3 hours
weigh the sample again by using analytical weighing balance i.e. the final
weight.
5.3.3.8
Note down readings
on given Annexure-1
5.3.4
Observation:
5.3.4.1
Maximum 0.5%.
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
5.0ml of 0.01M
hydrochloric acid.
5.4.2.2
50.0ml of ethanol
(96%).
5.4.2.3
0.1M sodium
hydroxide.
5.4.2.4
Thymolphthalein
solution (as indicator).
5.4.3
Sample:
5.4.3.1
0.250g.
5.4.4
Method
of analysis:
5.4.4.1 Take
a 100.0ml of beaker and take 0.250g of sample in it.
5.4.4.2 Add
a mixture of 50.0ml of ethanol (96%) and dissolve it by using magnetic stirrer
i.e. SOP.
5.4.4.3 Add
5.0ml of 0.01M hydrochloric acid, stir it again.
5.4.4.4 Fill
the right hand side burette with titrant 0.1M sodium hydroxide.
5.4.4.5 Carry
out a Potentiometric titration using thymolphthalein solution (as indicator).
5.4.4.6 Operate
potentiometer according to SOP.
5.4.4.7 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.
5.4.4.8 Plot
a graph, volume used v/s millivolts.
5.4.4.9 Find
out the END POINT. Read the volume added between the 2 points of inflexion.
5.4.4.10 Peak
of graph indicates END POINT i.e. the point at which maximum millivolts. Note
down volume used at that point.
5.4.4.11 Perform
blank titration without using sample. Similarly, as sample titration performed.
Record observations in annexure-2.
5.4.4.12 Calculate
volume used by substance by using formula:
Volume used by
substance = Blank titration - Sample titration.
5.4.4.13 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 sodium hydroxide is equivalent to 31.39mg of Venlafaxine hydrochloride C17H28ClNO2.
5.4.6
Limit:
5.4.6.1 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 / Venlafaxine
hydrochloride: 2015, pp. 1153-1154.
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 desiccator.
Annexure 2: Assay
observations and calculations (Potentiometric titration).
Annexure: 1
Observations
of percentage loss of drying by using desiccator
|
Percentage
loss of drying by using desiccator
Apparatus:
____________________
Temperature:
__________________
Weight
of Sample = _____________
Time
period = _____________
Pressure=
_________________
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
|
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