1.0 OBJECTIVE:
To
lay down a procedure for the active raw material of the Dapoxetine 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 Assay:
5.1.1
Apparatus:
5.1.1.1 Glassware (according to requirement).
5.1.1.2 Potentiometer.
5.1.2
Material and reagents:
5.1.2.1 10.0ml of anhydrous acetic acid.
5.1.2.2 0.1M Perchloric acid.
5.1.2.3 Crystal violet solution (as indicator).
5.1.3
Sample:
5.1.3.1 0.12g of Dapoxetine Hydrochloride.
5.1.4
Method of analysis:
5.1.4.1 Take a 100.0ml of beaker and add 0.12g of
sample in it.
5.1.4.2 Add 60.0ml of anhydrous acetic acid R in
it and dissolve by using magnetic stirrer i.e. SOP
5.1.4.3 Fill the right hand side burette with
titrant 0.1M Perchloric acid.
5.1.4.4 Carry out a Potentiometric titration using
crystal violet solution as an indicator.
5.1.4.5 Operate potentiometer according to SOP
5.1.4.6 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.
5.1.4.7 Plot a graph, volume used v/s millivolts.
5.1.4.8 Find out the END POINT.
5.1.4.9 Peak of graph indicates END POINT i.e. the
point at which maximum millivolts. Note down volume used at that point.
5.1.4.10 Perform blank titration without using
sample. Similarly, as sample titration performed. Record observations in annexure-1.
5.1.4.11 Calculate volume used by substance by
using formula:
Volume
used by substance = Blank titration - Sample titration.
5.1.4.12 Calculate percentage purity of the sample
by using formula:
%age
purity = volume used by substance x factor x 100
Weight of sample
5.1.5
Factor:
5.1.5.1 1ml of 0.1M Perchloric acid is equivalent
to 34.55mg of Dapoxetine
Hydrochloride.
5.1.6
Limit:
5.1.6.1 98.0% to 102.0% (anhydrous substance).
6.0 REVISION
LOG:
Revision No.
|
Effective Date
|
Reason
|
00
|
New
SOP
|
7.0 REFERENCES:
7.1 Manufacturer’s
specifications.
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
|
QCEO
|
Quality
control Equipment (Operation).
|
v/s
|
Verses
|
mV
|
Millivolts
|
g
|
Grams
|
ml
|
Milliliter
|
mg
|
Milligram
|
M
|
Molar
|
%
|
Percentage
|
R
|
Reagent
|