CITICHOLINE SODIUM SOP


CITICHOLINE SODIUM SOP

1.0  OBJECTIVE:
To lay down a procedure of analytical report for the active raw material of Citicholine sodium 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 crystals or a crystalline powder, odorless.
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        Chloroform.
5.1.2.1.3        Ethanol.
5.1.2.1.4        Acetone.
5.1.2.1.5        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 4 test tubes and add small quantity of sample for testing solubility according to B.P specifications.
5.1.2.3.2        Add chloroform in test tube 1, ethanol in test tube 2, acetone in test tube 3 and purified water 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 chloroform is insoluble.
5.1.2.4.2        The sample in test tube 2 containing with ethanol is insoluble.
5.1.2.4.3        The sample in test tube 3 containing with acetone is insoluble.
5.1.2.4.4        The sample in test tube 4 containing with purified water is freely soluble.
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  Desiccator.
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 desiccator apparatus with desiccant (phosphorous pentaoxide)
5.2.3.3  Place the sample into the china dish or petri dish and dry it.
5.2.3.4  Set the temperature 100oC under reduce pressure for at least 5 hours.
5.2.3.5  And wait till the sample loses its moisture.
5.2.3.6  After 5 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  Loses NMT6.0% of its weight.
5.3  Assay:
5.3.1        Apparatus:
5.3.1.1  UV/VIS Spectrophotometer.
5.3.1.2  Analytical weighing balance.
5.3.1.3  Glassware (according to the requirement).
5.3.1.4  Magnetic stirrer.
5.3.2        Material and reagents:
5.3.2.1  0.1N HCl.
5.3.2.2  200.0mg of citicholine sodium.
5.3.2.3  Purified water (q.s).
5.3.3        Blank solution:
5.3.3.1  0.1N HCl.
5.3.4        Sample solution:
5.3.4.1  Take a 100.0ml of volumetric flask and add 200.0mg of citicholine sodium in it.
5.3.4.2  Add sufficient quantity of 0.1N HCl. And sonicate to dissolve it by using Sonicator operates it.
5.3.4.3  And make up the final volume up to 100.0ml with the same solvent and mix it well again.
5.3.4.4  Filter the solution through filter paper.
5.3.4.5  Further dilute 1.0ml of filtrate to 100.0ml in another 100.0ml of volumetric flask with 0.1N HCl solution. And mix well by using magnetic stirrer operates it
5.3.5        Procedure:
5.3.5.1  Switch on the UV/VIS Spectrophotometer instrument as per SOP operate it i.e.
5.3.5.2  Allow to stabilize for 15min.
5.3.5.3  Set the desired wavelength i.e. 280nm with knob in increasing order.
5.3.5.4  Keep the sensitivity switch at the highest position.
5.3.5.5  Put the mode selector at %T position.
5.3.5.6  Set the filter wheel as per the wavelength.
5.3.5.7  Adjust zero percent transmittance with the help of set zero control.
5.3.5.8  Rinse reference cuvette and sample cuvette with blank solution 2 to 3 times.
5.3.5.9  Adjust 100% T with the help of % knob.
5.3.5.10       Remove the cuvette and drain out the blank solution from it. Rinse it with sample 2 to 3 times and filled with sample solution.
5.3.5.11    Clean the outer surface of the reference cuvette with tissue paper.
5.3.5.12    Place the cuvette into the sample holder and cover the cuvette compartment.
5.3.5.13    The reading show on the data position is the absorbance or %T of the sample.
5.3.5.14    Note down values in annexure-2.
5.3.5.15    Calculate the potency of citicholine sodium using the formula given below:
%age = sample absorbance × 510.32 × 1000 × 100 × 100
13000 × weight of sample × (100-LOD)
5.3.6        Limit:
5.3.6.1  Not less than 98.0% (on dried basis).
6.0  REVISION LOG:
Revision No.
Effective Date
Reason
00

New SOP

7.0  REFERENCES:
7.1  Manufacturer specifications.
8.0  ANNEXURES:
Annexure 1: Observations of Percentage Loss of drying by using desiccator.
Annexure 2: Observations and calculations of UV/VIS spectrophotometer.








Annexure: 1
Observations of percentage loss of drying by using desiccator
Percentage loss of drying by using desiccator
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
Observations and calculations of UV/VIS spectrophotometer
UV/VIS spectrophotometer
Model: _____________________________                             Date: _________________
OBSERVATIONS:
Thickness of cell:

Spectral range:

Maxima absorption wavelength

Sample:

Other reagent used:


No. of obs.
Concentration
Wavelength
Absorbance









CALCULATIONS:







Results: _______________
Remarks: ______________________________________________________________


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
ml
Milliliter
UV/VIS
Ultra violet/ Visible
nm
Nanometer
oC
Degree centigrade
%
Percentage
λ
Lambda
mg
Milligram
N
Normal
HCl
Hydrochloric acid
min
Minute
q.s.
Quantity sufficient
T
Transmittance
LOD
Loss on drying
g
Grams


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