CHONDROITIN SULFATE SODIUM SOP


CHONDROITIN SULFATE SODIUM SOP


1.0  OBJECTIVE:
To lay down a procedure for the active raw material of the Chondroitin Sulfate 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 or almost white.
5.1.1.2  Hygroscopic powder.
5.1.2        Solubility:
5.1.2.1  Material and equipment:
5.1.2.1.1        Glassware (2 test tubes, 1 spatula, 1 pipette).
5.1.2.1.2        Ethanol (96%).
5.1.2.1.3        Acetone.
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 a test tube 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 acetone in test tube 2 and observe.
5.1.2.3.4        Add Ethanol (96%) 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 freely soluble.
5.1.2.4.2        The sample in test tube 2 & 3 containing with acetone and Ethanol (96%) are practically insoluble respectively.
5.2  Solution S1:
5.2.1        Material and equipment:
5.2.1.1  Glassware (1 50.0ml of beaker, 1 spatula, 1 glass rod, 1 pipette).
5.2.1.2  Analytical weighing balance.
5.2.1.3  Magnetic stirrer.
5.2.1.4  Carbon-dioxide free water.
5.2.2        Sample:
5.2.2.1  2.5g.
5.2.3        Preparation of solution S:
5.2.3.1  Take a beaker of 50.0ml and add sample 2.5g in it.
5.2.3.2  Add in it 50.0ml of carbon-dioxide free water, dissolve by using magnetic stirrer operate.
5.3  Identification tests:
5.3.1        Sodium test:
5.3.1.1  Material and equipment:
5.3.1.1.1        Glassware (test tube, spatula, beaker, glass rod).
5.3.1.1.2        Analytical weighing balance.
5.3.1.1.3        Burner.
5.3.1.1.4        1.0ml of dilute ammonia.
5.3.1.1.5        Ice-water.
5.3.1.1.6        1.0ml of ammonium carbonate solution R.
5.3.1.2  Sample:
5.3.1.2.1        0.5ml of solution S1.
5.3.1.3  Method:
5.3.1.3.1        Take a test tube and add 0.5ml of solution S1.
5.3.1.3.2        Add 1.5ml of methoxyphenylacetic reagent R.
5.3.1.3.3        Cool in ice-water for 30min.
5.3.1.3.4        Observe the changes.
5.3.1.3.5        A voluminous, white, crystalline ppt is formed.
5.3.1.3.6        Place in purified water at 20oC and stir for 5minutes.
5.3.1.3.7        The ppt does not disappear.
5.3.1.3.8        Add 1.0ml of dilute ammonia.
5.3.1.3.9        The ppt dissolves completely.
5.3.1.3.10    Add 1.0ml of ammonium carbonate solution R.
5.3.1.3.11    Observe the changes.
5.3.1.4  Observations:
5.3.1.4.1        No ppt is formed.
5.4  Loss on drying:
5.4.1        Material and equipment:
5.4.1.1  Glassware (according to requirement).
5.4.1.2  Analytical weighing balance.
5.4.1.3  Oven.
5.4.2        Sample:
5.4.2.1  1.0g.
5.4.3        Method:
5.4.3.1  Weigh 1.0g of the test sample.
5.4.3.2  Set the oven apparatus.
5.4.3.3  Place the sample into the tray and dry it.
5.4.3.4  Set the temperature of oven at 105oC for at least 4hour.
5.4.3.5  And wait till the sample loses its moisture.
5.4.3.6  After 4 hours weigh the sample again by using analytical weighing balance i.e. the final weight.
5.4.3.7  Note down readings on given Annexure-1.
5.4.4        Observation:
5.4.4.1  Maximum 12.0%.
5.5  Assay:
5.5.1        Apparatus:
5.5.1.1  Glassware (according to requirement).
5.5.1.2  Titration apparatus.
5.5.1.3  Magnetic stirrer.
5.5.2        Material and reagents:
5.5.2.1  0.1g of chondroitin sulfate sodium CRS.
5.5.2.2  4.0g cetylpyridinium chloride monohydrate.
5.5.2.3  0.1ml of a 1% solution of methylene blue R.
5.5.2.4  Purified water.
5.5.3        Sample:
5.5.3.1  0.1g.
5.5.4        Method of analysis:
5.5.4.1  Test solution (a):
5.5.4.1.1        Take a 100.0ml of beaker and add weighed 0.1g (m1) of the substance in it.
5.5.4.1.2        Dissolve it in sufficient quantity of purified water.
5.5.4.1.3        Finally dilute it to 100.0ml with the same solvent.
5.5.4.2  Reference solution (a):
5.5.4.2.1        Take a 100.0ml of beaker and add weighed 0.1g (m0) of chondroitin sulfate sodium CRS, previously dried as described in the test for loss on drying in 5.4 point in it.
5.5.4.2.2        Dissolve it in sufficient quantity of purified water.
5.5.4.2.3        Finally dilute it to 100.0ml with the same solvent.
5.5.4.3  Titrant solution (a):
5.5.4.3.1        Take a 1000.0ml of beaker and add weighed 4.0g cetylpyridinium chloride monohydrate R in it.
5.5.4.3.2        Dissolve it in sufficient quantity of purified water.
5.5.4.3.3        Finally dilute it to 1000.0ml with purified water.
5.5.4.4  Visual titration:
5.5.4.4.1        Set titration apparatus.
5.5.4.4.2        Fill the right hand side burette with titrant solution (a).
5.5.4.4.3        Take 40.0ml of test solution (a) in volumetric flask and titrate it with titrant solution (a).
5.5.4.4.4        The solution becomes turbid.
5.5.4.4.5        At the end point, the liquid appears clear, with an almost-white ppt in suspension.
5.5.4.4.6        The ppt is more apparent if 0.1ml of a 1% solution of methylene blue R is added before starting the titration.
5.5.4.4.7        The precipitated particles are more apparent against the blue background.
5.5.4.4.8        Similarly, take 40.0ml of reference solution (a) in volumetric flask and titrate it with titrant solution (a).
5.5.4.4.9        Note down the volume used as shown in Annexure-2.
5.5.4.5  Calculate the percentage content of chondroitin sulfate sodium using the following expression:
     u1 x m0    x      100       x     Z
                                                       u0 x m1           100-h
u0= volume of appropriate titrant solution when titrating the appropriate reference solution, in milliliters.
u1= volume of appropriate titrant solution when titrating the appropriate test solution, in milliliters.
h= loss on drying of the substance to be examined, as a percentage.
Z= percentage content of H2O (C14H19NNa2O14S)x in chondroitin sulfate sodium CRS.
5.5.5        Limit:
5.5.5.1  95.0% to 105.0% (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 /Chondroitin sulfate sodium: 2015, pp. 538-541.
7.2  The British Pharmacopoeia. Vol V., Official Monograph /Qualitative Reactions and Tests: 2015, pp. 266-270.
8.0  ANNEXURES:
Annexure 1: Observations of percentage loss of drying.
Annexure 2: Observations and calculations of assay of Chondroitin sulfate sodium.









Annexure: 1
Observations of percentage loss of drying
Percentage loss of drying
Apparatus: ____________________
Temperature: __________________
Pressure: _____________________
Weight of Sample = _____________
Time period = _____________
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 assay of Chondroitin sulfate sodium
VISUAL TITRATION
Indicator:____________________________
Weight of sample( m1):_____________________                          
Weight of reference material (m0):____________
Titrant:______________________________
Percentage content of H2O (C14H19NNa2O14S)x in chondroitin sulfate sodium CRS (Z):________________________
Sample titration
Sr.#
Initial volume (vi)
(ml)
Final volume (vf)
(ml)
u1=vf-vi
(ml)
1.



2.



3.



Average volume (u1): _________________
Blank titration
Sr.#
Initial volume (vi)
(ml)
Final volume (vf)
(ml)
u0=vf-vi
(ml)
1.



2.



3.



Average volume(u0): _________________




Calculations:
Calculate the percentage content of chondroitin sulfate sodium using the following expression:

     u1 x m0    x      100       x     Z
                               u0 x m1           100-h





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
%
Percentage
R
Reagent
BP
British Pharmacopoeia
vi
Initial volume
vf
Final volume
h
Hour
oC
Degree centigrade


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