PIROXICAM METHOD OF ANALYSIS SOP


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.
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:
Sr.#
Volume used
(ml)
Voltmeter
(mV)












Plot a graph, volume used v/s millivolts and find out peak of graph i.e. END POINT of blank titration.
Sample titration:
Sr.#
Volume used
(ml)
Voltmeter
(mV)












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
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


No comments:

Post a Comment