CHLOROQUINE PHOSPHATE SOP


CHLOROQUINE PHOSPHATE SOP

1.0  OBJECTIVE:
To lay down a procedure for the active raw material of the Chloroquine Phosphate 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  Crystalline powder.
5.1.1.3  Hygroscopic.
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        Alcohol.
5.1.2.1.3        Methanol.
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 alcohol in test tube 2 and observe.
5.1.2.3.4        Add methanol 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 alcohol and methanol is very slightly soluble respectively.
5.2  Identification tests:
5.2.1        UV/VIS absorption Spectrophotometry:
5.2.1.1  Material and equipment:
5.2.1.1.1        UV/VIS Spectrophotometer.
5.2.1.1.2        Glassware (according to requirement).
5.2.1.1.3        Purified water.
5.2.1.2  Sample:
5.2.1.2.1        0.100g.
5.2.1.3  Method:
5.2.1.3.1        Test solution:
5.2.1.3.1.1  Take a beaker of 100.0ml and add 0.100g of sample in it.
5.2.1.3.1.2  Dissolve it in sufficient quantity of purified water.
5.2.1.3.1.3  And dilute it to 100.0ml with the same solvent.
5.2.1.3.1.4  Take another beaker and add 1.0ml of this solution in it.
5.2.1.3.1.5  Dilute it to 100.0ml with purified water.
5.2.1.3.2        Spectral range:
5.2.1.3.2.1  Examined between 210nm and 370nm.
5.2.1.3.3        Absorption maxima:
5.2.1.3.3.1  At 220nm, 235nm, 256nm, 329nm and 342nm.
5.2.1.3.4        Operate the UV/VIS spectrophotometer.
5.2.1.3.5        Examined between 210nm and 370nm the solution absorption maxima at 220nm, 235nm, 256nm, 329nm and 342nm.
5.2.1.3.6        Note down values of absorbance in annexure-1.
5.2.1.3.7        Calculate the specific absorbance by using formula:
1cmA1% = __a__
                                            b.c
5.2.1.4  Observations:
5.2.1.4.1        Specific absorbance:
5.2.1.4.1.1  The specific absorbances at the maxima are respectively 600 to 660, 350 to 390, 300 to 330, 325 to 355 and 360 to 390.
5.2.2        Melting point determination:
5.2.2.1  Material and equipment:
5.2.2.1.1        Glassware (according to requirement).
5.2.2.1.2        Melting point apparatus.
5.2.2.1.3        Capillary tubes.
5.2.2.1.4        Purified water.
5.2.2.2  Sample:
5.2.2.2.1        25.0mg.
5.2.2.3  Method:
5.2.2.3.1        Take a 50.0ml of beaker and add 25.0mg of sample in it.
5.2.2.3.2        Add 20.0ml of purified water and 8.0ml of picric acid solution R1.
5.2.2.3.3        The ppt, washed with purified water R, with alcohol R and finally with methylene chloride R.
5.2.2.3.4        Introduce the sufficient quantity of sample into a capillary tube.
5.2.2.3.5        Set the apparatus and immerse the capillary tube into the apparatus such that the closed end is near the center of the bulb of thermometer.
5.2.2.3.6        Switch on the melting point apparatus.
5.2.2.3.7        Operate the melting point apparatus.
5.2.2.3.8        Raise the temperature of the apparatus.
5.2.2.3.9        Record the temperature at which the last particle passes into the liquid phase.
5.2.2.3.10    Record measurements in annexure-2.
5.2.2.4  Observations:
5.2.2.4.1        The melting point is 206oC-209oC.
5.2.3        Phosphates determination test:
5.2.3.1  Material and equipment:
5.2.3.1.1        Glassware (1 test tube, 1 pipette).
5.2.3.1.2        Analytical weighing balance.
5.2.3.1.3        10.0ml of purified water.
5.2.3.1.4        2.0ml of dilute sodium hydroxide solution R.
5.2.3.1.5        Methylene chloride.
5.2.3.1.6        Nitric acid.
5.2.3.1.7        2.0ml of molybdovanadic reagent R.
5.2.3.2  Sample:
5.2.3.2.1        0.1g.
5.2.3.3  Method:
5.2.3.3.1        Take a test tube and add 0.1g of sample in it.
5.2.3.3.2        Add 10.0ml of purified water R and 2.0ml of dilute sodium hydroxide solution R. Dissolve it by using magnetic stirrer.
5.2.3.3.3        Shake with 2 quantities, each of 20.0ml, of methylene chloride R.
5.2.3.3.4        The aqueous layer is extracted, acidified it by addition of nitric acid R.
5.2.3.3.5        Take 1.0ml of the above prescribed solution and add 2.0ml of molybdovanadic reagent R
5.2.3.3.6        Observe the changes.
5.2.3.4  Observations:
5.2.3.4.1        A yellow 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.
5.3.3.3  Place the sample into the tray and dry it.
5.3.3.4  Set the temperature of oven at 105oC 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 2.0%.
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  50.0ml of anhydrous acetic acid.
5.4.2.2  0.1M Perchloric acid.
5.4.2.3  Crystal violet solution (as indicator).
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 50.0ml of anhydrous acetic acid in it and dissolve it by using magnetic stirrer.
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.
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 25.79mg of Chloroquine phosphate C18H32ClN3O8P2.
5.4.6        Limit:
5.4.6.1  98.5% 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 /Chloroquine Phosphate: 2015, pp. 521.
8.0  ANNEXURES:
Annexure 1: Observations and Calculations of UV/VIS spectrophotometer.
Annexure 2: Observations of Melting point apparatus.
Annexure 3: Observations of Percentage Loss of drying by using oven.
Annexure 4: Assay observations and calculations (Potentiometric titration).













Annexure: 1
Observations and Calculations of UV/VIS spectrophotometer
UV/VIS spectrophotometer
Model: _____________________________                             Date: _________________
OBSERVATIONS:
No. of tablets:

Sample:

Thickness of cell (b):

Concentration solution (c):

At A(1%, 1cm):

Wavelength (λ):


No. of obs.
Concentration
(c)
Wavelength
(λ)
Absorbance
(a)
Specific absorbance
A (1%,1cm)










CALCULATIONS:
1cmA1% = __a__
                                         b.c





Results: _______________
Remarks: ______________________________________________________________

Annexure: 2
Observations of Melting point apparatus
Sample = _____________
Time period = _____________
Sr.#
Initial (Ti)
(oC)
Final (Tf)
(oC)
Tf - Ti
(oC)












Average: _____________

Result: _________________

Remarks: _______________________________________________________________













Annexure: 3
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: 4
Assay observations and calculations (Potentiometric titration)
Potentiometric titration
Reference electrode: ___________________
Indicator electrode: ____________________
Speed of magnetic stirrer: _______________
Titrant used: __________________________
Indicator: ____________________________
Blank titration:
Sr.#
Volume used
(ml)
Voltmeter
(mV)












Plot a graph, volume used v/s millivolts and find out peak of graph i.e. END POINT of blank titration.
Sample titration:
Sr.#
Volume used
(ml)
Voltmeter
(mV)












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
%
Percentage
B.P
British pharmacopoeia
ml
Milliliter
oC
Degree centigrade
mg
Milligram
g
Grams
M
Molar
Min
Minutes
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
R
Reagent
λ
Lambda


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