VILDAGLIPTIN METHOD OF ANALYSIS SOP
1.0 OBJECTIVE:
To
lay down a procedure for the active raw material of the Vildagliptin 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 Vildagliptin.
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 No. BM/QCEO/SOP007-00.
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 30.61mg of Vildagliptin.
5.1.6
Limit:
5.1.6.1
99.0% to 101.0%
(anhydrous substance).
6.0 REVISION LOG:
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Revision No.
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Effective Date
|
Reason
|
|
00
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|
New SOP
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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: ____________________________________________________________
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9.0 ABBREVIATIONS:
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Abbreviation
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Expanded Form
|
|
SOP
|
Standard
operating procedure
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|
&
|
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
|