PIROXICAM
METHOD OF ANALYSIS SOP
1.0 OBJECTIVE:
To
lay down a procedure of analytical report for the active raw material of
Piroxicam 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 slightly
yellow.
5.1.1.2
Crystalline
powder.
5.1.2
Solubility:
5.1.2.1
Material and equipment:
5.1.2.1.1
Glassware (3 test
tubes, spatula).
5.1.2.1.2
Purified water.
5.1.2.1.3
Methylene
chloride.
5.1.2.1.4
Anhydrous ethanol.
5.1.2.2
Sample:
5.1.2.2.1
Small quantity.
5.1.2.3
Method:
5.1.2.3.1
Take 3 test tubes
and add small quantity of sample for testing solubility according to B.P
specifications.
5.1.2.3.2
Add purified
water, methylene chloride and anhydrous ethanol in each test tube separately in
a small volume and observe the solubility of the sample.
5.1.2.4
Observations:
5.1.2.4.1
The sample in test
tube 1 containing with water is practically insoluble.
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 containing with anhydrous ethanol is slightly soluble.
5.2 Assay:
5.2.1
Apparatus:
5.2.1.1
Glassware
(according to requirement).
5.2.1.2
Potentiometer.
5.2.2
Material
and reagents:
5.2.2.1
Acetic hydride.
5.2.2.2
Anhydrous acetic
acid.
5.2.2.3
0.1M Perchloric
acid.
5.2.2.4
Crystal violet
solution.
5.2.3
Sample:
5.2.3.1
0.250g.
5.2.4
Method
of analysis:
5.2.4.1 Take
a 100.0ml of beaker and take 0.250g of sample in it.
5.2.4.2 Add
60.0ml of a mixture of equal volumes of acetic anhydride and anhydrous acetic
acid.
5.2.4.3 Fill
the right hand side burette with titrant 0.1M Perchloric acid.
5.2.4.4 Carry
out a Potentiometric titration using crystal violet solution as an indicator.
5.2.4.5 Operate
potentiometer according to SOP No. BM/QCEO/SOP036-00.
5.2.4.6 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.
5.2.4.7 Plot
a graph, volume used v/s millivolts.
5.2.4.8 Find
out the END POINT.
5.2.4.9 Peak
of graph indicates END POINT i.e. the point at which maximum millivolts. Note
down volume used at that point.
5.2.4.10 Perform
blank titration without using sample. Similarly, as sample titration performed.
Record observations in annexure-1.
5.2.4.11 Calculate
volume used by substance by using formula:
Volume
used by substance = Blank titration - Sample titration.
5.2.4.12 Calculate
percentage purity of the sample by using formula:
%age
purity = volume used by substance x factor x 100
Weight
of sample
5.2.5
Factor:
5.2.5.1 1ml
of 0.1M Perchloric acid is equivalent to 33.14mg of Piroxicam C15H13N3O4S.
5.2.6
Limit:
5.2.6.1
98.5% to 101.0%
(dried substance).
6.0 REVISION LOG:
|
Revision No.
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Effective Date
|
Reason
|
|
00
|
|
New SOP
|
7.0 REFERENCES:
7.1
The British
Pharmacopoeia. Vol II.,
Official Monograph /Piroxicam: 2015, pp. 598-600.
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:
|
Abbreviation
|
Expanded Form
|
|
SOP
|
Standard
operating procedure
|
|
&
|
And
|
|
No.
|
Number
|
|
Ltd.
|
Limited
|
|
Q.C
|
Quality
control
|
|
B.P
|
British
pharmacopoeia
|
|
M
|
Molar
|
|
g
|
Grams
|
|
ml
|
Milliliter
|
|
mg
|
Milligram
|
|
%
|
Percentage
|
|
Vol
|
Volume
|
|
QCA
|
Quality
control active ingredient
|
|
F
|
Format
|
|
mV
|
Millivolts
|
|
v/s
|
Verses
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