ISONIAZID SOP


1.0  OBJECTIVE:
To lay down a procedure of analytical report for the active raw material of the Isoniazid from the Pharmacopoeial specifications.
2.0  SCOPE:
This SOP shall be applicable in Q.C laboratory.
3.0  RESPONSIBILITY:
3.1  Q.C Analysts.
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  Colourless crystals.
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        Alcohol.
5.1.2.1.3        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 2 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.
5.1.2.4  Observations:
5.1.2.4.1        The sample in test tube 1 containing with water is freely soluble.
5.1.2.4.2        The sample in test tube 2 containing with alcohol is sparingly soluble.
5.2  Identification tests:
5.2.1        Melting point determination:
5.2.1.1  Material and equipment:
5.2.1.1.1        Glassware (according to requirement).
5.2.1.1.2        Melting point apparatus.
5.2.1.1.3        Capillary tubes.
5.2.1.1.4        Purified water.
5.2.1.2  Sample:
5.2.1.2.1        Sufficient quantity of sample.
5.2.1.3  Method:
5.2.1.3.1        Introduce the sufficient quantity of sample into a capillary tube.
5.2.1.3.2        Set the apparatus and immerse the capillary tube into the apparatus such that the closed end is near the centre of the bulb of thermometer.
5.2.1.3.3        Switch on the melting point apparatus.
5.2.1.3.4        Operate the melting point apparatus according to the SOP.
5.2.1.3.5        Raise the temperature of the apparatus.
5.2.1.3.6        Record the temperature at which the last particle passes into the liquid phase.
5.2.1.3.7        Record measurements in annexure-1.
5.2.1.4  Observations:
5.2.1.4.1        The melting point is 170oC-174oC.
5.2.2         
5.2.2.1  Material and equipment:
5.2.2.1.1        Glassware (1 test tube, 1 glass rod, 1 pipette).
5.2.2.1.2        Melting point apparatus.
5.2.2.1.3        2.0ml of purified water.
5.2.2.1.4        10.0ml of a warm 10g/L solution of vanillin R.
5.2.2.1.5        5.0ml of alcohol (70% v/v) R.
5.2.2.2  Sample:
5.2.2.2.1        0.1g.
5.2.2.3  Method:
5.2.2.3.1        Take a test tube add in it 0.1g of the sample in it.
5.2.2.3.2        Add 2.0ml of purified water in it. Dissolve it thoroughly. And add 10.0ml of a warm 10g/L solution of vanillin R.
5.2.2.3.3        Allow it to stand and scratch the wall of the test tube with a glass rod.
5.2.2.3.4        Observe the changes.
5.2.2.3.5        A yellow ppt is formed.
5.2.2.3.6        Add 5.0ml of alcohol (70% v/v) R. Observe changes again.
5.2.2.3.7        It recrystallizes.
5.2.2.3.8        Dry it in oven at 100oC to 105oC.
5.2.2.3.9        Introduce the sufficient quantity of sample into a capillary tube.
5.2.2.3.10    Set the apparatus and immerse the capillary tube into the apparatus such that the closed end is near the centre of the bulb of thermometer.
5.2.2.3.11    Switch on the melting point apparatus.
5.2.2.3.12    Operate the melting point apparatus according to the SOP.
5.2.2.3.13    Raise the temperature of the apparatus.
5.2.2.3.14    Record the temperature at which the last particle passes into the liquid phase.
5.2.2.3.15    Record measurements in annexure-2.
5.2.2.4  Observations:
5.2.2.4.1        It melts at 226oC to 231oC.
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 105oC 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-3.
5.3.4        Observation:
5.3.4.1  Not more than 0.1%.
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  20.0ml of hydrochloric acid.
5.4.2.2  0.2g of potassium bromide R.
5.4.2.3  0.05ml of methyl red solution R as an indicator.
5.4.2.4  Purified water.
5.4.2.5  0.0167M Potassium bromate.
5.4.3        Sample:
5.4.3.1  0.250g.
5.4.4        Method of analysis:
5.4.4.1  Sample titration:
5.4.4.1.1        Take a 100.0ml of beaker and 0.250g of sample in it.
5.4.4.1.2        Add sufficient quantity of purified water in it and dissolve by using magnetic stirrer operate according to SOP.
5.4.4.1.3        Dilute it to 100.0ml with the same solvent.
5.4.4.1.4        Take 20.0ml of the solution in conical flask and add 100.0ml of purified water, 20.0ml of hydrochloric acid and 0.2g of potassium bromide R.
5.4.4.1.5        Set titration apparatus.
5.4.4.1.6        Use 0.05ml of methyl red solution as an indicator.
5.4.4.1.7        Titrate with 0.0167M Potassium bromate.
5.4.4.1.8        Add dropwise titrant shake continuously, until the red colour disappears.
5.4.4.1.9        Note down the volume used as shown in Annexure-4.
5.4.4.1.10    And take average.
5.4.4.2  Blank titration:
5.4.4.2.1        Take 20.0ml of the solution in conical flask and add 100.0ml of purified water, 20.0ml of hydrochloric acid and 0.2g of potassium bromide R.
5.4.4.2.2        Set titration apparatus.
5.4.4.2.3        Use 0.05ml of methyl red solution as an indicator.
5.4.4.2.4        Titrate with 0.0167M Potassium bromate.
5.4.4.2.5        Add dropwise titrant shake continuously, until the red colour disappears.
5.4.4.2.6        Note down the volume used as shown in Annexure-4.
5.4.4.2.7        And take average.
5.4.4.3  Calculate percentage purity.
5.4.4.4  Calculations:
5.4.4.4.1        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.
5.4.4.4.2        For percentage purity use formula:
%age purity = volume used by substance x factor x 100
                                                                              Weight of sample
5.4.4.4.3        Put values and calculate %age purity.
5.4.5        Factor:
5.4.5.1  1ml of 0.0167M Potassium bromate is equivalent to 3.429mg of C6H7N3O.
5.4.6        Limit:
5.4.6.1  99.0% to 101.0%.
6.0  REVISION LOG:
Revision No.
Effective Date
Reason
00

New SOP

7.0  REFERENCES:
7.1  The British Pharmacopoeia. Vol I., Official Monograph / Isoniazid: 2015, pp. 262.
8.0  ANNEXURES:
Annexure 1: Observations of Melting point apparatus.
Annexure 2: Observations of Melting point apparatus.
Annexure 3: Observations of Percentage Loss of drying by using oven.
Annexure 4: Observations and calculation of titration.
Annexure: 1
Observations of Melting point apparatus
Sample = _____________
Time period = _____________
Sr.#
Initial (Ti)
(oC)
Final (Tf)
(oC)
Tf - Ti
(oC)












Average: _____________

Result: _________________

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
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: 4
Observations and calculation of titration.
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
Q.C
Quality control
%
Percentage
B.P
British pharmacopoeia
mg
Milligram
ml
Milliliter
ppt
Precipitate
g
Grams
M
Molar
Vol
Volume
QCA
Quality control active ingredient
F
Format
oC
Degree centigrade
R
Reagent
vi
Initial volume
vf
Final volume


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