PREGABALIN METHOD OF ANALYSIS SOP


1.0  OBJECTIVE:
To lay down a procedure for the active raw material of the Pregabalin 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  A white crystalline solid.
5.2  Identification test:
5.2.1        Melting point determination:
5.2.1.1  Material and equipment:
5.2.1.1.1        Glassware (according to requirement).
5.2.1.1.2        Melting point apparatus.
5.2.1.1.3        Capillary tubes.
5.2.1.1.4        Purified water.
5.2.1.2  Sample:
5.2.1.2.1        Sufficient quantity of sample.
5.2.1.3  Method:
5.2.1.3.1        Introduce the sufficient quantity of sample into a capillary tube.
5.2.1.3.2        Set the apparatus and immerse the capillary tube into the apparatus such that the closed end is near the center of the bulb of thermometer.
5.2.1.3.3        Switch on the melting point apparatus.
5.2.1.3.4        Operate the melting point apparatus according to the SOP No. BM/QCEO/SOP009-00.
5.2.1.3.5        Raise the temperature of the apparatus.
5.2.1.3.6        Record the temperature at which the last particle passes into the liquid phase.
5.2.1.3.7        Record measurements in annexure-1.
5.2.1.4  Observations:
5.2.1.4.1        The melting point is 186oC-188oC. (7.1)
5.3  Assay:
5.3.1        Apparatus:
5.3.1.1  Glassware (according to requirement).
5.3.1.2  Potentiometer.
5.3.2        Material and reagents:
5.3.2.1  80.0ml of anhydrous acetic acid.
5.3.2.2  5.0ml of acetic acid.
5.3.2.3  0.1M Perchloric acid.
5.3.2.4  Crystal violet solution (as indicator).
5.3.3        Sample:
5.3.3.1  0.200g.
5.3.4        Method of analysis:
5.3.4.1  Take a 100.0ml of beaker and add 0.200g of sample in it.
5.3.4.2  Add 80.0ml of anhydrous acetic acid in it and dissolve by using magnetic stirrer i.e. SOP.
5.3.4.3  Add 5.0ml of acetic acid and dissolve by using magnetic stirrer for at least 10min.
5.3.4.4  Fill the right hand side burette with titrant 0.1M Perchloric acid.
5.3.4.5  Carry out a Potentiometric titration using crystal violet solution as an indicator.
5.3.4.6  Operate potentiometer according to SOP.
5.3.4.7  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.
5.3.4.8  Plot a graph, volume used v/s millivolts.
5.3.4.9  Find out the END POINT.
5.3.4.10    Peak of graph indicates END POINT i.e. the point at which maximum millivolts. Note down volume used at that point.
5.3.4.11    Perform blank titration without using sample. Similarly, as sample titration performed. Record observations in annexure-2.
5.3.4.12    Calculate volume used by substance by using formula:
Volume used by substance = Blank titration - Sample titration.
5.3.4.13    Calculate percentage purity of the sample by using formula:
%age purity = volume used by substance x factor x 100
                                                   Weight of sample
5.3.5        Factor:
5.3.5.1  1ml of 0.1M Perchloric acid is equivalent to 16.16mg of Pregabalin C8H17NO2.
5.3.6        Limit:
5.3.6.1  99.0% to 100.0%. (7.2)
6.0  REVISION LOG:
Revision No.
Effective Date
Reason
00

New SOP

7.0  REFERENCES:
7.1  A.C. Moffat, M.D. Osselton and B. Widdop. Vol-2, Part-2/ Monographs: Pregabalin in Clarke’s Analysis of Drugs and Poisons. Pharmaceutical press. 4th edition, 2011.
7.2  Manufacturer specifications.
8.0  ANNEXURES:
Annexure 1: Observations of Melting point apparatus.
Annexure 2: Assay observations and calculations (Potentiometric titration).

                                                                 



Annexure: 1
Observations of Melting point apparatus
Sample = _____________
Time period = _____________
Sr.#
Initial (Ti)
(oC)
Final (Tf)
(oC)
Tf - Ti
(oC)












Average: _____________

Result: _________________

Remarks: _______________________________________________________________












                                                           


                                                            Annexure: 2
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
QCA
Quality control active ingredient
F
Format
Q.C
Quality control
Vol
Volume
g
Grams
ml
Milliliter
oC
Degree centigrade
mg
Milligram
M
Molar
%
Percentage
v/s
Verses
mV
Millivolts
g
Grams
ml
Milliliter
Ti
Initial temperature
Tf
Final temperature
Temp.
Temperature


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