MEPYRAMINE MALEATE SOP
1.0 OBJECTIVE:
To
lay down a procedure for the active raw material of the Mepyramine maleate 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
yellowish.
5.1.1.2
Crystalline
powder.
5.1.2
Solubility:
5.1.2.1
Material and equipment:
5.1.2.1.1
Glassware (2 test
tubes, 1 spatula).
5.1.2.1.2
Ethanol (96%).
5.1.2.1.3
Purified water.
5.1.2.2
Sample:
5.1.2.2.1
Small quantity.
5.1.2.3
Method:
5.1.2.3.1
Take 2 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 Ethanol (96%) in
test tube 2 and observe.
5.1.2.4
Observations:
5.1.2.4.1
The sample in test
tube 1 containing with purified water is very soluble.
5.1.2.4.2
The sample in test
tube 2 containing with ethanol (96%) is freely 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
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 centre 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.
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 99oC-103oC.
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
0.01M hydrochloric
acid.
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 0.01M hydrochloric acid.
5.2.2.3.1.3 And
dilute it to 100.0ml with the same acid.
5.2.2.3.1.4 Take
1.0ml of this solution in 100.0ml of beaker.
5.2.2.3.1.5 And
dilute it to 100.0ml with 0.01M hydrochloric acid.
5.2.2.3.2
Spectral
range:
5.2.2.3.2.1 220-350nm.
5.2.2.3.3
Absorption
maxima:
5.2.2.3.3.1 The
solution shows 2 absorption maxima 239nm and 316nm.
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 239nm and 316nm.
5.2.2.3.6
Note down values
of absorbance in annexure-2.
5.2.2.3.7
Calculate the specific
absorbances at the absorption maxima by using formula:
1cmA1% = __a__
b.c
5.2.2.4
Observations:
5.2.2.4.1
Specific
absorbance at 239nm:
5.2.2.4.1.1 431
to 477.
5.2.2.4.2
Specific
absorbance at 316nm:
5.2.2.4.2.1 196
to 220.
5.2.3
5.2.3.1
Material and equipment:
5.2.3.1.1
Glassware (2 test
tubes, 1 pipette, 1 spatula).
5.2.3.1.2
Analytical
weighing balance.
5.2.3.1.3
Water-bath.
5.2.3.1.4
Vortex mixer.
5.2.3.1.5
Mortar and pestle.
5.2.3.1.6
1.0ml of strong
sodium hydroxide solution.
5.2.3.1.7
Ether.
5.2.3.1.8
Resorcinol.
5.2.3.1.9
Sulfuric acid.
5.2.3.1.10 1.0ml
of bromine water.
5.2.3.1.11 Purified
water.
5.2.3.2
Sample:
5.2.3.2.1
0.1g.
5.2.3.3
Method:
5.2.3.3.1
Take mortar and
pestle and add 0.1g of sample in it and add 3.0ml of purified water and 1.0ml
of strong sodium hydroxide solution with the help of pipette, and triturate it.
5.2.3.3.2
Take sample in
test tube and shake with 3 quantities each of 5.0ml of ether.
5.2.3.3.3
Take 0.1ml of
aqueous layer in another test tube A after separating layers.
5.2.3.3.4
Add a solution of
10.0mg of resorcinol in 3.0ml of sulfuric acid.
5.2.3.3.5
Heat it on
water-bath for 15min, observe change.
5.2.3.3.6
No colour
develops.
5.2.3.3.7
To the rest of the
aqueous layer in another test tube B add 1.0ml of bromine water.
5.2.3.3.8
Heat on water-bath
for 15min and then heat to boiling and cool it.
5.2.3.3.9
Take 0.2ml of this
solution in another test tube C.
5.2.3.3.10 Add
a solution of 10.0mg of resorcinol in 3.0ml of sulfuric acid.
5.2.3.3.11 Heat
it on water-bath for 15min and observe the changes.
5.2.3.4
Observations:
5.2.3.4.1
A violet-pink
colour develops.
5.3 Loss
on drying:
5.3.1
Material and equipment:
5.3.1.1
Glassware
(according to requirement).
5.3.1.2
Analytical
weighing balance.
5.3.1.3
Oven.
5.3.2
Sample:
5.3.2.1
1.0g.
5.3.3
Method:
5.3.3.1
Weigh 1.0g of the
test sample.
5.3.3.2
Set the oven
apparatus. Operate it according to the SOP.
5.3.3.3
Place the sample
into the tray and dry it.
5.3.3.4
Set the
temperature of oven at 80oC for 45min.
5.3.3.5
And wait till the
sample loses its moisture.
5.3.3.6
After 45min weigh
the sample again by using analytical weighing balance i.e. the final weight.
5.3.3.7
Note down readings
on given Annexure-3.
5.3.4
Observation:
5.3.4.1
Maximum 0.25%.
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
40.0ml of
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
0.15g.
5.4.4
Method
of analysis:
5.4.4.1 Take
a 50.0ml of beaker and take 0.15g of sample in it.
5.4.4.2 Add
40.0ml of anhydrous acetic acid in it and dissolve by using magnetic stirrer
i.e. 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-4.
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-4.
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 20.07mg of Mepyramine maleate C21H27N3O5.
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 II.,
Official Monograph /Mepyramine maleate: 2015, pp. 217-218.
8.0 ANNEXURES:
Annexure 1: Observations
of Melting point apparatus.
Annexure 2: Observations
of UV/VIS spectrophotometer.
Annexure 3: Observations
of Percentage Loss of drying by using oven.
Annexure 4: 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:
1cmA1%
= __a__
b.c
Results:
_______________
Remarks:
______________________________________________________________
|
Annexure: 3
Observations
of percentage loss of drying by using Oven
|
Percentage
loss of drying by using Oven
Apparatus:
___________________
Temperature:
__________________
Weight
of Sample = _____________
Time
period = _____________
Pressure=
_________________
Average % Loss of Moisture: _____________
Remarks:
_______________________________________________________________
|
||||||||||||||||||||||||
Annexure:
4
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
|
|
QCA
|
Quality
control active ingredient
|
|
F
|
Format
|
|
Q.C
|
Quality
control
|
|
Vol
|
Volume
|
|
mg
|
Milligram
|
|
ml
|
Milliliter
|
|
ppt
|
Precipitate
|
|
M
|
Molar
|
|
g
|
Grams
|
|
Min
|
Minute
|
|
%
|
Percentage
|
|
Ti
|
Initial
temperature
|
|
Tf
|
Final
temperature
|
|
Temp.
|
Temperature
|
|
v/s
|
Verses
|
|
mV
|
Millivolts
|
|
oC
|
Degree
centigrade
|
|
R
|
Reagent
|
|
λ
|
Lambda
|
|
UV/VIS
|
Ultraviolet/
visible
|
|
nm
|
Nanometer
|
|
Hrs.
|
Hours
|
|
A
|
Absorbance
|
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