ATENOLOL SOP



ATENOLOL SOP


1.0  OBJECTIVE:
To lay down a procedure for analytical report of the active raw material Atenolol from the Pharmacopoeial specifications.
2.0  SCOPE:
This SOP shall be applicable in Q.C laboratory.
3.0  RESPONSIBILITY:
3.1  Q.C Analysts.
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 (3 test tubes, 1 spatula).
5.1.2.1.2        Ethanol (96%).
5.1.2.1.3        Purified water.
5.1.2.1.4        Methylene chloride.
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 in test tube 1 and observe.
5.1.2.3.3        Add anhydrous ethanol in test tube 2 and observe.
5.1.2.3.4        Add methylene chloride in test tube 3 and observe.
5.1.2.4  Observations:
5.1.2.4.1        The sample in test tube 1 containing with purified water is sparingly soluble.
5.1.2.4.2        The sample in test tube 2 containing with anhydrous ethanol is soluble.
5.1.2.4.3        The sample in test tube 3 containing with methylene chloride is slightly soluble.
5.2  Identification tests:
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        Burner.
5.2.1.1.5        Desiccator.
5.2.1.1.6        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        Unless otherwise prescribed, dry the finely powdered substance in vacuo and over the anhydrous silica gel for 24 hrs.
5.2.1.3.2        Introduce the sufficient quantity of sample into a capillary tube.
5.2.1.3.3        Set the apparatus and immerse the capillary tube into the apparatus such that the closed end is near the centre of the bulb of thermometer.
5.2.1.3.4        Switch on the melting point apparatus.
5.2.1.3.5        Operate the melting point apparatus according to the SOP No. .
5.2.1.3.6        Raise the temperature of the apparatus.
5.2.1.3.7        Record the temperature at which the last particle passes into the liquid phase.
5.2.1.3.8        Record measurements in annexure-1.
5.2.1.4  Observations:
5.2.1.4.1        The melting point is 152oC-155oC.
5.2.2        UV/VIS absorption Spectrophotometry:
5.2.2.1  Material and equipment:
5.2.2.1.1        UV/VIS Spectrophotometer.
5.2.2.1.2        Glassware (according to requirement).
5.2.2.1.3        Methanol.
5.2.2.2  Sample:
5.2.2.2.1        0.1g.
5.2.2.3  Method:
5.2.2.3.1        Test solution:
5.2.2.3.1.1  Take a beaker of 100.0ml and add 0.1g of sample in it.
5.2.2.3.1.2  Dissolve it in sufficient quantity of methanol.
5.2.2.3.1.3  And dilute it to 100.0ml with the same solvent.
5.2.2.3.1.4  Take another beaker of 100.0ml and suck 10.0ml of the above solution in it.
5.2.2.3.1.5  Dilute it again to 100.0ml with methanol.
5.2.2.3.2        Spectral range:
5.2.2.3.2.1  230-350nm.
5.2.2.3.3        Absorption maxima:
5.2.2.3.3.1  At 275nm and 282nm.
5.2.2.3.4        Operate the UV/VIS spectrophotometer according to the SOP.
5.2.2.3.5        Measure the absorbance of the resulting solution at the maximum wavelength 275nm and 282nm.
5.2.2.3.6        Note down values of absorbance in annexure-2.
5.2.2.3.7        Calculate the absorbance ratio A275/A282.
5.2.2.4  Observations:
5.2.2.4.1        Absorbance ratio A275/A282:
5.2.2.4.1.1  1.15 to 1.20.
5.3  Other tests:
5.3.1        Solution S:
5.3.1.1  Material and equipment:
5.3.1.1.1        Glassware (1 beaker, 1 stirrer, 1 spatula).
5.3.1.1.2        Analytical weighing balance.
5.3.1.2  Sample:
5.3.1.2.1        0.1g.
5.3.1.3  Preparation of solution S:
5.3.1.3.1        Take a beaker of 50.0ml and add 0.1g of sample in it.
5.3.1.3.2        Add approximately 5ml of purified water in it and dissolve it by using magnetic stirrer operate according to SOP.
5.3.1.3.3        Finally dilute it to 10.0ml with the same solvent.
5.3.2        Optical rotation:
5.3.2.1  Material and equipment:
5.3.2.1.1        Glassware (according to the requirement).
5.3.2.1.2        Polarimeter.
5.3.2.2  Sample:
5.3.2.2.1        Solution S.
5.3.2.3  Method:
5.3.2.3.1        Operate the Polarimeter according to SOP.
5.3.2.3.2        Determine optical rotation on the solution S.
5.3.2.3.3        Fill the Polarimeter tube with blank solution and determine the observed optical rotation.
5.3.2.3.4        Similarly, fill the Polarimeter tube with sample solution and determine the observed optical rotation.
5.3.2.3.5        Note down the values in annexure-3.
5.3.2.4  Observation:
5.3.2.4.1        +0.10o to -0.10o.
5.3.3        Loss on drying:
5.3.3.1  Material and equipment:
5.3.3.1.1        Glassware (according to requirement).
5.3.3.1.2        Hot air oven.
5.3.3.1.3        Analytical weighing balance.
5.3.3.2  Sample:
5.3.3.2.1        1.0g.
5.3.3.3  Method:
5.3.3.3.1        Weigh 1.0g of the test sample.
5.3.3.3.2        Set the Hot air oven apparatus.
5.3.3.3.3        Operate the Hot air oven according to the SOP.
5.3.3.3.4        Place the sample into the tray.
5.3.3.3.5        Set the temperature of oven at 105oC for at least 45 minutes.
5.3.3.3.6        And wait till the sample loses its moisture.
5.3.3.3.7        After 45 minutes weigh the sample again by using analytical weighing balance i.e. the final weight.
5.3.3.3.8        Note down readings on given Annexure-4
5.3.3.4  Observations:
5.3.3.4.1        Maximum 0.5%.
5.4  Assay:
5.4.1        Apparatus:
5.4.1.1  Glassware (according to requirement).
5.4.1.2  Potentiometer.
5.4.1.3  Magnetic stirrer.
5.4.2        Material and reagents:
5.4.2.1  Anhydrous acetic acid.
5.4.2.2  0.1M Perchloric acid.
5.4.2.3  Crystal violet solution.
5.4.3        Sample:
5.4.3.1  0.200g.
5.4.4        Method of analysis:
5.4.4.1  Take a 100.0ml of beaker and take 0.200g of sample in it.
5.4.4.2  Add 80.0ml of anhydrous acetic acid in it and dissolve it by using magnetic stirrer operate according to SOP.
5.4.4.3  Fill the right hand side burette with titrant 0.1M Perchloric acid.
5.4.4.4  Carry out a Potentiometric titration using crystal violet solution as an indicator.
5.4.4.5  Operate potentiometer according to SOP.
5.4.4.6  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-5.
5.4.4.7  Plot a graph, volume used v/s millivolts.
5.4.4.8  Find out the END POINT.
5.4.4.9  Peak of graph indicates END POINT i.e. the point at which maximum millivolts. Note down volume used at that point.
5.4.4.10    Perform blank titration without using sample. Similarly, as sample titration performed. Record observations in annexure-5.
5.4.4.11    Calculate volume used by substance by using formula:
Volume used by substance = Blank titration - Sample titration.
5.4.4.12    Calculate percentage purity of the sample by using formula:
%age purity = volume used by substance x factor x 100
                       Weight of sample
5.4.5        Factor:
5.4.5.1  1ml of 0.1M Perchloric acid is equivalent to 26.63mg of Atenolol C14H22N2O3.
5.4.6        Limit:
5.4.6.1  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 I., Official Monograph /Atenolol: 2015, pp. 205-206.


8.0  ANNEXURES:
Annexure 1: Observations of Melting point apparatus.
Annexure 2: Observations and calculations of UV/VIS Spectrophotometer.
Annexure 3: Observations of Optical rotation.
Annexure 4: Observations of Percentage Loss of drying by using Hot air oven.
Annexure 5: 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
Observations and Calculations of UV/VIS spectrophotometer
UV/VIS spectrophotometer
Model: _____________________________                             Date: _________________
OBSERVATIONS:
Thickness of cell:

Spectral range:
230-350nm.
Maxima absorption wavelength:
275nm and 282nm.
Sample:

Other reagent used:


No. of obs.
Concentration
Wavelength
Absorbance









CALCULATIONS:
Absorbance ratio A275/A282 =



Results: _______________
Remarks: ______________________________________________________________


Annexure: 3
Observations of Optical rotation
Determination of Optical rotation
Instrument: ___________________                                              Date: _______________
Model: _______________________        Length of Polarimeter tube: ________________
Sample: ________________________________g.
Solvent: ________________________________ml.
Concentration of sample solution: ____________g/ml.
Blank solution:
Sr.#
Blank solution
Temperature
Optical rotation
(α)












                                                                                                 Average: _______________
Optical rotation of blank solution: _______________
Sample solution:
Sr.#
Sample solution
Temperature
Optical rotation
(α)












                                                                                                 Average: _______________
Optical rotation of sample solution: ______________
Optical rotation of substance = Blank solution - Sample solution.

                                                                      Result: ________________
Remarks: ___________________________________________________________

Annexure: 4
Observations of percentage loss of drying by using Hot air oven
Percentage loss of drying by using Hot air oven
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: 5
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
Sr.#
Serial number
Q.C
Quality control
%
Percentage
B.P
British pharmacopoeia
g
Grams
ml
Milliliter
oC
Degree centigrade
mg
Milligram
nm
Nanometer
M
Molar
h
Hour
Vol
Volume
vi
Initial volume
vf
Final volume
QCA
Quality control active ingredient
F
Format
Ti
Initial temperature
Tf
Final temperature
Temp.
Temperature
v/s
Verses
mV
Millivolts
UV/VIS
Ultraviolet/ visible
o
Degree (angle)
l
Length
c
Concentration (g/ml)
g/ml
Gram per milliliter
α
Alpha
λ
Lambda


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