RISPERIDONE METHOD OF ANALYSIS SOP


1.0  OBJECTIVE:
To lay down a procedure of analytical report for the active raw material of Risperidone 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 almost white powder.
5.1.2        Solubility:
5.1.2.1  Material and equipment:
5.1.2.1.1        Glassware (4 test tubes, spatula).
5.1.2.1.2        Purified water.
5.1.2.1.3        Methylene chloride.
5.1.2.1.4        Ethanol (96%).
5.1.2.1.5        Dilute acid solution (e.g. dilute HNO3).
5.1.2.2  Sample:
5.1.2.2.1        Small quantity.
5.1.2.3  Method:
5.1.2.3.1        Take 4 test tubes and add small quantity of sample for testing solubility according to B.P specifications.
5.1.2.3.2        Add purified water in test tube 1, Methylene chloride in test tube 2, ethanol (96%) in test tube 3, dilute acid solution like HNO3 in test tube 4 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 purified water is practically insoluble.
5.1.2.4.2        The sample in test tube 2 containing with Methylene chloride is freely soluble.
5.1.2.4.3        The sample in test tube 3 containing with ethanol (96%) is sparingly soluble.
5.1.2.4.4        The sample in test tube 4 containing with dilute acid solution like HNO3 is dissolved.
5.2  Loss on drying:
5.2.1        Material and equipment:
5.2.1.1  Glassware (according to requirement).
5.2.1.2  Analytical weighing balance.
5.2.1.3  Oven.
5.2.2        Sample:
5.2.2.1  1.0g.
5.2.3        Method:
5.2.3.1  Weigh 1.0g of the test sample.
5.2.3.2  Set the oven apparatus. Operate it according to the SOP.
5.2.3.3  Place the sample into the tray and dry it.
5.2.3.4  Set the temperature of oven at 105oC for at least 4 hours.
5.2.3.5  And wait till the sample loses its moisture.
5.2.3.6  After 4 hours weigh the sample again by using analytical weighing balance i.e. the final weight.
5.2.3.7  Note down readings on given Annexure-1.
5.2.4        Observation:
5.2.4.1  Maximum 0.5%.
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  1 volume of anhydrous acetic acid.
5.3.2.2  7 volumes of methyl ethyl ketone.
5.3.2.3  0.1M Perchloric acid.
5.3.2.4  Crystal violet solution.
5.3.3        Sample:
5.3.3.1  0.160g.
5.3.4        Method of analysis:
5.3.4.1  Take a 100.0ml of beaker and take 0.160g of sample in it.
5.3.4.2  Add 70.0ml of a mixture of 1 volume of anhydrous acetic acid and 7 volumes of methyl ethyl ketone. Dissolve it by using magnetic stirrer i.e..
5.3.4.3  Fill the right hand side burette with titrant 0.1M Perchloric acid.
5.3.4.4  Carry out a Potentiometric titration using crystal violet solution as an indicator.
5.3.4.5  Operate potentiometer according to SOP
5.3.4.6  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-2.
5.3.4.7  Plot a graph, volume used v/s millivolts.
5.3.4.8  Find out the END POINT.
5.3.4.9  Peak of graph indicates END POINT i.e. the point at which maximum millivolts. Note down volume used at that point.
5.3.4.10    Perform blank titration without using sample. Similarly, as sample titration performed. Record observations in annexure-2.
5.3.4.11    Calculate volume used by substance by using formula:
Volume used by substance = Blank titration - Sample titration.
5.3.4.12    Calculate percentage purity of the sample by using formula:
%age purity = volume used by substance x factor x 100
                           Weight of sample
5.3.5        Factor:
5.3.5.1  1ml of 0.1M Perchloric acid is equivalent to 20.53mg of Risperidone C23H27FN4O2.
5.3.6        Limit:
5.3.6.1  99.0% 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 /Risperidone: 2015, pp. 756-758.
8.0  ANNEXURES:
Annexure 1: Observations of Percentage Loss of drying by using oven.
Annexure 2: Assay observations and calculations (Potentiometric titration).



Annexure: 1
Observations of percentage loss of drying by using Oven
Percentage loss of drying by using Oven
Apparatus: ____________________
Temperature: __________________
Weight of Sample = _____________
Time period = _____________
Pressure= _________________
Sr.#
Time (min)
Weight of sample (g)
% Loss of Moisture
Initial weight
Final weight















Average % Loss of Moisture: _____________

% Loss of Moisture:






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
Q.C
Quality control
B.P
British pharmacopoeia
M
Molar
g
Grams
ml
Milliliter
mg
Milligram
%
Percentage
h
Hours
Vol
Volume
QCA
Quality control active ingredient
F
Format
mV
Millivolts
v/s
Verses
kPa
Kilo Pascal
Min
Minutes


No comments:

Post a Comment