MAGALDRATE SOP

1.0  OBJECTIVE:
To lay down a procedure for the active raw material of the Magaldrate from the Pharmacopoeia 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.
5.1.2        Solubility:
5.1.2.1  Material and equipment:
5.1.2.1.1        Glassware (3 test tubes, 1 spatula, 1 pipette).
5.1.2.1.2        Ethanol (96%).
5.1.2.1.3        Purified water.
5.1.2.1.4        Dilute mineral acid.
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 dilute mineral acid in test tube 3 and observe.
5.1.2.4  Observations:
5.1.2.4.1        The sample in test tube 1 & 2 containing with purified water and ethanol (96%) is practically insoluble.
5.1.2.4.2        The sample in test tube 3 containing with dilute mineral acid is soluble.
5.2  Identification tests:
5.2.1         
5.2.1.1  Material and equipment:
5.2.1.1.1        Glassware (1 test tube, 1 pipette, 1 funnel).
5.2.1.1.2        Burner.
5.2.1.1.3        Filter paper.
5.2.1.1.4        20.0ml of 3M hydrochloric acid.
5.2.1.1.5        Purified water.
5.2.1.1.6        Dilute ammonia R1.
5.2.1.1.7        2.0ml of ammonium chloride solution.
5.2.1.1.8        2.0g of ammonium carbonate.
5.2.1.1.9        Disodium hydrogen phosphate solution.
5.2.1.2  Sample:
5.2.1.2.1        0.6g.
5.2.1.3  Method:
5.2.1.3.1        Take a beaker of 100.0ml and add 0.6g of sample in it.
5.2.1.3.2        Dissolve the sample in 20.0ml of 3M hydrochloric acid.
5.2.1.3.3        And then add about 30.0ml of purified water, heat on burner till boiling.
5.2.1.3.4        Adjust to pH 6.2 with dilute ammonia R1, and again continue boiling on burner for further 2 min.
5.2.1.3.5        Filter it by using filtration apparatus.
5.2.1.3.6        Retain the ppt and filtrate.
5.2.1.3.7        Take 2.0ml of filtrate in a test tube add 2.0ml of ammonium chloride solution and neutralize with a solution prepared by dissolving 2.0g of ammonium carbonate and 2.0ml of dilute ammonia R1in 20.0ml of purified water.
5.2.1.3.8        Observe the changes.
5.2.1.3.9        No ppt is produced.
5.2.1.3.10    Add Disodium hydrogen phosphate solution and observe the changes.
5.2.1.4  Observations:
5.2.1.4.1        A white, crystalline ppt is produced which does not dissolve in dilute ammonia R1.
5.2.2        Aluminium test:
5.2.2.1  Material and equipment:
5.2.2.1.1        Glassware (1 test tube, 1 pipette).
5.2.2.1.2        0.5ml of dilute hydrochloric acid.
5.2.2.1.3        0.5ml of thioacetamide reagent.
5.2.2.1.4        Dilute sodium hydroxide.
5.2.2.1.5        Ammonium chloride solution.
5.2.2.2  Sample:
5.2.2.2.1        Ppt retained in identification test 5.2.1.
5.2.2.3  Method:
5.2.2.3.1        Take 2.0ml of the sample (i.e. ppt retained in identification test 5.2.1.) and add about 0.5ml of dilute hydrochloric acid and about 0.5ml of thioacetamide reagent. Dissolve it.
5.2.2.3.2        Observe the changes.
5.2.2.3.3        No ppt is formed.
5.2.2.3.4        Add drop-wise dilute sodium hydroxide solution.
5.2.2.3.5        Observe the changes.
5.2.2.3.6        A gelatinous white ppt is formed.
5.2.2.3.7        When further dilute sodium hydroxide solution is added, gelatinous white ppt is dissolved.
5.2.2.3.8        Gradually add ammonium chloride solution.
5.2.2.3.9        Observe the changes.
5.2.2.4  Observations:
5.2.2.4.1        The gelatinous white ppt is re-formed.
5.2.3        Sulfates test:
5.2.3.1  Material and equipment:
5.2.3.1.1        Glassware (according to requirement).
5.2.3.1.2        1.0ml of dilute hydrochloric acid.
5.2.3.1.3        1.0ml of barium chloride solution R1.
5.2.3.2  Sample:
5.2.3.2.1        Filtrate retained in identification test 5.2.1
5.2.3.3  Method:
5.2.3.3.1        Take a test tube add in it 5.0ml of sample with the help of pipette.
5.2.3.3.2        Add 1.0ml of dilute hydrochloric acid and 1.0ml of barium chloride solution R1.
5.2.3.3.3        Observe the changes.
5.2.3.4  Observations:
5.2.3.4.1        A white ppt is formed.
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 200oC for at least 4h.
5.3.3.5  And wait till the sample loses its moisture.
5.3.3.6  After 4h weigh the sample again by using analytical weighing balance i.e. the final weight.
5.3.3.7  Note down readings on given Annexure-1.
5.3.4        Observation:
5.3.4.1  10.0% to 20.0%.
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 1.0M hydrochloric acid.
5.4.2.2  0.1M sodium hydroxide.
5.4.3        Sample:
5.4.3.1  1.5g.
5.4.4        Method of analysis:
5.4.4.1  Take a 100.0ml of beaker and take 1.5g of sample in it.
5.4.4.2  Add 50.0ml of 1.0M hydrochloric acid, dissolve by using magnetic stirrer i.e. SOP.
5.4.4.3  Fill the right hand side burette with titrant 1.0M sodium hydroxide.
5.4.4.4  Carry out a Potentiometric titration of excess hydrochloric acid to pH 3.0.
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-2.
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-2.
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 1.0M hydrochloric acid is equivalent to 35.40mg of Magaldrate Al5Mg10(OH)31(SO4)2.
5.4.6        Limit:
5.4.6.1  90.0% 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 II., Official Monograph /Magaldrate: 2015, pp. 159-160.
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 by using oven.
Annexure 2: Assay observations and calculations (Potentiometric titration).








Annexure: 1
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: 2
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
QCA
Quality control active ingredient
F
Format
Q.C
Quality control
Vol
Volume
Ti
Initial temperature
Tf
Final temperature
Temp.
Temperature
v/s
Verses
mV
Millivolts
g
Grams
ml
Milliliter
Min
Minutes
oC
Degree centigrade
mg
Milligram
M
Molar
%
Percentage
R
Reagent


No comments:

Post a Comment