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:
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:
Average: _______________
Optical
rotation of blank solution: _______________
Sample solution:
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=
_________________
Average
% 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:
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: ____________________________________________________________
|
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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