CHOLINE THEOPHYLLINATE SOP

CHOLINE THEOPHYLLINATE SOP


1.0  OBJECTIVE:
To lay down a procedure for the active raw material of the Choline theophyllinate 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 Manger.
5.0  PROCEDURE:
5.1  Characters:
5.1.1        Appearance:
5.1.1.1  White, crystalline 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        Ether.
5.1.2.1.4        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 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 Ethanol (96%) in test tube 2 and observe.
5.1.2.3.4        Add ether 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 very soluble.
5.1.2.4.2        The sample in test tube 2 containing with Ethanol (96%) is soluble.
5.1.2.4.3        The sample in test tube 3 containing with ether is very slightly soluble.
5.2  Identification tests:
5.2.1        UV/VIS absorption Spectrophotometry:
5.2.1.1  Material and equipment:
5.2.1.1.1        Glassware (according to requirement).
5.2.1.1.2        UV/VIS Spectrophotometer.
5.2.1.1.3        0.1M sodium hydroxide.
5.2.1.2  Sample:
5.2.1.2.1        0.002% w/v solution in 0.1M sodium hydroxide.
5.2.1.3  Spectral range:
5.2.1.3.1        230-350nm.
5.2.1.4  Absorption maxima:
5.2.1.4.1        At 275nm.
5.2.1.5  Test solution:
5.2.1.5.1        Take a beaker of 100.0ml and prepare a sample solution 0.002% w/v solution in 0.1M sodium hydroxide.
5.2.1.6  Method:
5.2.1.6.1        Switch ON the UV/VIS spectrophotometer and operate it .
5.2.1.6.2        Observe the test solution on above given spectral range.
5.2.1.6.3        Note down the absorbance at maxima λ i.e. 275nm.
5.2.1.6.4        Observe the absorbance at 275nm and note it down in annexure-1.
5.2.1.7  Observation:
5.2.1.7.1        The absorbance at 275nm is about 0.83.
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.
5.3.3.3  Place the sample into the tray.
5.3.3.4  Set the temperature of oven at 105oC and dry it to constant weight for at least 45 minutes.
5.3.3.5  And wait till the sample loses its moisture.
5.3.3.6  After 45 minutes weigh the sample again by using analytical weighing balance i.e. the final weight.
5.3.3.7  Note down readings on given Annexure-2
5.3.4        Observation:
5.3.4.1  Losses not more than 0.5% of its weight.
5.4  Assay:
5.4.1        For choline:
5.4.1.1  Apparatus:
5.4.1.1.1        Glassware (according to requirement).
5.4.1.1.2        Titration apparatus.
5.4.1.1.3        Magnetic stirrer.
5.4.1.2  Material and reagents:
5.4.1.2.1        Methyl red mixed solution (as indicator).
5.4.1.2.2        0.05M sulfuric acid VS.
5.4.1.2.3        50.0ml of Purified water.
5.4.1.3  Sample:
5.4.1.3.1        0.6g.
5.4.1.4  Method of analysis:
5.4.1.4.1        Sample titration:
5.4.1.4.1.1  Take a flask and add 0.6g of sample in it.
5.4.1.4.1.2  Dissolve it in 50.0ml of Purified water by using magnetic stirrer operate
5.4.1.4.1.3  Add few drops of Methyl red mixed solution (as indicator).
5.4.1.4.1.4  Set titration apparatus.
5.4.1.4.1.5  Titrate with 0.05M sulfuric acid VS until a violet end point is obtained.
5.4.1.4.1.6  Note down the volume used as shown in Annexure-3.
5.4.1.4.1.7  Take 3 readings at least and take average.
5.4.1.4.2        Blank titration:
5.4.1.4.2.1  Take a flask and add 50.0ml of Purified water in it.
5.4.1.4.2.2  Add few drops of Methyl red mixed solution (as indicator).
5.4.1.4.2.3  Set titration apparatus.
5.4.1.4.2.4  Titrate with 0.05M sulfuric acid VS until a violet end point is obtained.
5.4.1.4.2.5  Note down the volume used as shown in Annexure-3.
5.4.1.4.2.6  Take 3 readings at least and take average.
5.4.1.4.3        Calculate percentage purity.
5.4.1.4.4        Calculations:
5.4.1.4.4.1  After taking average volume of both blank titration and sample titration. Calculate the volume used by the examined substance by using formula:
Volume used by substance = Blank titration - Sample titration.
5.4.1.4.4.2  For percentage purity use formula:
%age purity = volume used by substance x factor x 100
                                                                              Weight of sample
5.4.1.4.4.3  Put values and calculate %age purity.
5.4.1.5  Factor:
5.4.1.5.1        1ml of 0.05M sulfuric acid VS is equivalent to 12.12mg of choline C5H15NO2.
5.4.1.6  Limit:
5.4.1.6.1        41.9% to 43.6% (dried substance).
5.4.2        For theophylline:
5.4.2.1  Apparatus:
5.4.2.1.1        Glassware (according to requirement).
5.4.2.1.2        Titration apparatus.
5.4.2.1.3        Ice.
5.4.2.1.4        Water-bath.
5.4.2.1.5        Magnetic stirrer.
5.4.2.2  Material and reagents:
5.4.2.2.1        25.0ml of 0.1M silver nitrate VS.
5.4.2.2.2        0.1M sodium hydroxide VS.
5.4.2.2.3        Purified water.
5.4.2.3  Sample:
5.4.2.3.1        Solution obtained in assay of choline.
5.4.2.4  Method of analysis:
5.4.2.4.1        Sample titration:
5.4.2.4.1.1  Take a flask and add solution obtained from assay of choline.
5.4.2.4.1.2  Add 25.0ml of 0.1M silver nitrate VS and warm it on water-bath for 15min.
5.4.2.4.1.3  Allow it to cool in ice for 30min, containing in a beaker of 1000.0ml.
5.4.2.4.1.4  After that filter it by using filtration apparatus.
5.4.2.4.1.5  Finally wash the residue with 10.0ml quantity of purified water 3 times.
5.4.2.4.1.6  Set titration apparatus.
5.4.2.4.1.7  Titrate the combined filtrate and washings with 0.1M sodium hydroxide VS.
5.4.2.4.1.8  Note down the volume used as shown in Annexure-3.
5.4.2.4.1.9  Take 3 readings at least and take average.
5.4.2.4.2        Blank titration:
5.4.2.4.2.1  Take a flask and add blank solution obtained from assay of choline (i.e. blank titration).
5.4.2.4.2.2  Add 25.0ml of 0.1M silver nitrate VS and warm it on water-bath for 15min.
5.4.2.4.2.3  Allow it to cool in ice for 30min, containing in a beaker of 1000.0ml.
5.4.2.4.2.4  After that filter it by using filtration apparatus.
5.4.2.4.2.5  Finally wash the residue with 10.0ml quantity of purified water 3 times.
5.4.2.4.2.6  Set titration apparatus.
5.4.2.4.2.7  Titrate the combined filtrate and washings with 0.1M sodium hydroxide VS.
5.4.2.4.2.8  Note down the volume used as shown in Annexure-3.
5.4.2.4.2.9  Take 3 readings at least and take average.
5.4.2.4.3        Calculate percentage purity.
5.4.2.4.4        Calculations:
5.4.2.4.4.1  After taking average volume of both blank titration and sample titration. Calculate the volume used by the examined substance by using formula:
Volume used by substance = Blank titration - Sample titration.
5.4.2.4.4.2  For percentage purity use formula:
%age purity = volume used by substance x factor x 100
                                                                            Weight of sample
5.4.2.4.4.3  Put values and calculate %age purity.
5.4.2.5  Factor:
5.4.2.5.1        1ml of 0.1M sodium hydroxide is equivalent to 18.02mg of C7H8N4O2.
5.4.2.6  Limit:
5.4.2.6.1        61.7% to 65.5% (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 / Choline Theophyllinate: 2015, pp. 538.
8.0  ANNEXURES:
Annexure 1: Observations of UV/VIS spectrophotometer.
Annexure 2: Observations of Percentage Loss of drying by using oven.
Annexure 3: Observations and calculations of for choline assay.
Annexure 4: Observations and calculations for theophylline assay.














Annexure: 1
Observations of UV/VIS spectrophotometer
UV/VIS spectrophotometer
Model: _____________________________                             Date: _________________
OBSERVATIONS:
Thickness of cell:

Spectral range:
230-350nm.
Maximum wavelength absorbance at
275nm.
Sample:

Other reagent used:


No. of obs.
Concentration
Wavelength
Absorbance














Results: _______________
Remarks: ______________________________________________________________




Annexure: 2
Observations of percentage loss of drying by using Oven
Percentage loss of drying by using 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: 3
Observations and calculations for choline assay
Indicator: ___________________
Weight of sample: ____________                                                Factor: _____________
Titrant: _____________________
Sample titration
Sr.#
Initial volume (vi)
(ml)
Final volume (vf)
(ml)
vf-vi
(ml)
1.



2.



3.



Average volume: _________________
Blank titration
Sr.#
Initial volume (vi)
(ml)
Final volume (vf)
(ml)
vf-vi
(ml)
1.



2.



3.



Average volume: _________________
Calculations:
Volume used by substance = Blank titration - Sample titration.

%age purity = volume used by substance x factor x 100
                                                                     Weight of sample

Result: ____________________________________________________________________

Annexure: 4
Observations and calculations for theophylline assay
Indicator: ___________________
Weight of sample: ____________                                                Factor: _____________
Titrant: _____________________
Sample titration
Sr.#
Initial volume (vi)
(ml)
Final volume (vf)
(ml)
vf-vi
(ml)
1.



2.



3.



Average volume: _________________
Blank titration
Sr.#
Initial volume (vi)
(ml)
Final volume (vf)
(ml)
vf-vi
(ml)
1.



2.



3.



Average volume: _________________
Calculations:
Volume used by substance = Blank titration - Sample titration.

%age purity = volume used by substance x factor x 100
                                                                     Weight of sample

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
Min
Minutes
oC
Degree centigrade
mg
Milligram
M
Molar
vi
Initial volume
vf
Final volume
%
Percentage
R
Reagent
λ
Lambda
UV/VIS
Ultraviolet/ visible
w/v
Weight by volume
nm
Nanometer


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