DEXTROMETHORPHAN HYDROBROMIDE SOP



DEXTROMETHORPHAN HYDROBROMIDE SOP

1.0  OBJECTIVE:
To lay down a procedure for the active raw material of the Dextromethorphan hydrobromide 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  Almost white, crystalline powder.
5.1.2        Solubility:
5.1.2.1  Material and equipment:
5.1.2.1.1        Glassware (2 test tubes, 1 spatula).
5.1.2.1.2        Ethanol (96%).
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 Ethanol (96%) in test tube 2 and observe.
5.1.2.4  Observations:
5.1.2.4.1        The sample in test tube 1 containing with purified water is sparingly soluble.
5.1.2.4.2        The sample in test tube 2 containing with Ethanol (96%) is freely soluble.
5.2  Identification tests:
5.2.1        Specific optical rotation:
5.2.1.1  Material and equipment:
5.2.1.1.1        Polarimeter.
5.2.1.1.2        Analytical weighing balance.
5.2.1.1.3        Glassware (1 beaker of 50.0ml, 1 stirrer, 1 spatula, 1 glass rod).
5.2.1.1.4        0.1Mhydrochloric acid.
5.2.1.2  Sample:
5.2.1.2.1        0.2g.
5.2.1.3  Method:
5.2.1.3.1        Take a beaker of 50.0ml and add 0.2g of sample in it.
5.2.1.3.2        Dissolve it in 0.1Mhydrochloric acid (approx. 5.0ml) by using glass rod.
5.2.1.3.3        Dilute it to 10.0ml with the same acid.
5.2.1.3.4        Firstly clean the Polarimeter with clean dry cloth, according to SOP
5.2.1.3.5        Operate the Polarimeter according to SOP
5.2.1.3.6        Fill the Polarimeter tube with blank solution and determine the observed optical rotation.
5.2.1.3.7        Similarly, fill the Polarimeter tube with sample solution and determine the observed optical rotation.
5.2.1.3.8        Note down the values in annexure-1.
5.2.1.3.9        Calculate the specific optical rotation by using formula:
[α]λ T = α/lc
5.2.1.4  Observations:
5.2.1.4.1        -32.5 to -35.5.
5.2.2        Bromides test:
5.2.2.1  Material and equipment:
5.2.2.1.1        Glassware (according to requirement).
5.2.2.1.2        Centrifuge machine.
5.2.2.1.3        Dilute nitric acid.
5.2.2.1.4        Purified water.
5.2.2.1.5        0.4ml of Silver nitrate R1.
5.2.2.1.6        1.5ml of Ammonia.
5.2.2.2  Sample:
5.2.2.2.1        Quantity of substance to be examined equivalent to about 3.0mg of bromide.
5.2.2.3  Method:
5.2.2.3.1        Take a test tube add in it 2.0ml of water with the help of pipette.
5.2.2.3.2        Dissolve in 2.0ml of water a quantity of the substance to be equivalent to about 3.0mg of bromide.
5.2.2.3.3        Acidify with dilute nitric acid.
5.2.2.3.4        And add 0.4ml of silver nitrate R1.
5.2.2.3.5        Shake and allow it to stand.
5.2.2.3.6        A curdled, pale yellow ppt is formed.
5.2.2.3.7        Centrifuge it in centrifugation machine, according to SOP.
5.2.2.3.8        The obtained ppt is wash with 3 times 1.0ml quantities of purified water.
5.2.2.3.9        Carry out this operation rapidly is subdued light, degrading the fact that the supernatant solution may not become perfectly clear.
5.2.2.3.10    Suspend the precipitate in 2.0ml of water and add 1.5ml of ammonia.
5.2.2.3.11    Observe the changes.
5.2.2.4  Observations:
5.2.2.4.1        The precipitate dissolves with difficulty.
5.3  Assay:
5.3.1        Apparatus:
5.3.1.1  Glassware (according to requirement).
5.3.1.2  Potentiometer.
5.3.1.3  Magnetic stirrer.
5.3.2        Material and reagents:
5.3.2.1  5.0ml of 0.01M hydrochloric acid.
5.3.2.2  20.0ml of ethanol (96%).
5.3.2.3  0.1M sodium hydroxide.
5.3.2.4  Thymolphthalein solution (as indicator).
5.3.3        Sample:
5.3.3.1  0.3g.
5.3.4        Method of analysis:
5.3.4.1  Take a 100.0ml of beaker and take 0.3g of sample in it.
5.3.4.2  Add a mixture of 5.0ml of 0.01M hydrochloric acid and 20.0ml of ethanol (96%) dissolve by using magnetic stirrer.
5.3.4.3  Fill the right hand side burette with titrant 0.1M sodium hydroxide.
5.3.4.4  Carry out a Potentiometric titration using thymolphthalein solution (as indicator).
5.3.4.5  Operate potentiometer according to SOP.
5.3.4.6  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.
5.3.4.7  Plot a graph, volume used v/s millivolts.
5.3.4.8  Find out the END POINT. Read the volume added between the 2 points of inflexion.
5.3.4.9  Peak of graph indicates END POINT i.e. the point at which maximum millivolts. Note down volume used at that point.
5.3.4.10    Perform blank titration without using sample. Similarly, as sample titration performed. Record observations in annexure-2.
5.3.4.11    Calculate volume used by substance by using formula:
Volume used by substance = Blank titration - Sample titration.
5.3.4.12    Calculate percentage purity of the sample by using formula:
%age purity = volume used by substance x factor x 100
                          Weight of sample
5.3.5        Factor:
5.3.5.1  1ml of 0.1M sodium hydroxide is equivalent to 35.23mg of dextromethorphan hydrobromide C18H26BrNO.
5.3.6        Limit:
5.3.6.1  99.0% to 101.0% (anhydrous 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 / Dextromethorphan hydrobromide: 2015, pp. 714-716.
7.2  The British Pharmacopoeia. Vol V., Official Monograph /Qualitative Reactions and Tests: 2015, pp. 266-270.
8.0  ANNEXURES:
Annexure 1: Specific optical rotation observations and calculations.
Annexure 2: Assay observations and calculations (Potentiometric titration).





Annexure: 1
Specific optical rotation observations and calculations
Specific optical rotation
Instrument: ___________________                                              Date: _______________
Model: _______________________        Length of Polarimeter tube: ________________
Sample: ________________________________g.
Solvent: ________________________________ml.
Concentration of sample solution: ____________g/ml.
Blank solution:
Sr.#
Blank solution
Temperature
Optical rotation
(α)












                                                                                                 Average: _______________
Optical rotation of blank solution: _______________
Sample solution:
Sr.#
Sample solution
Temperature
Optical rotation
(α)












                                                                                                 Average: _______________
Optical rotation of sample solution: ______________
Optical rotation of substance = Blank solution - Sample solution.


Specific optical rotation of sample solution by using formula:
[α]λ T = α/lc






                                                                      Result: ________________
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
%
Percentage
B.P
British pharmacopoeia
g
Grams
ml
Milliliter
oC
Degree centigrade
mg
Milligram
g
Grams
M
Molar
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
o
Degree (angle)
l
Length
c
Concentration (g/ml)
g/ml
Gram per milliliter
α
Alpha
λ
Lambda
g/L
Grams per liter


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