BAMBUTEROL HYDROCHLORIDE SOP


BAMBUTEROL HYDROCHLORIDE SOP

1.0  OBJECTIVE:
To lay down a procedure of analytical report for the active raw material of the Bambuterol Hydrochloride 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.
5.1.2        Solubility:
5.1.2.1  Material and equipment:
5.1.2.1.1        Glassware (test tubes, 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 water is freely soluble.
5.1.2.4.2        The sample in test tube 2 containing with ethanol (96%) is soluble.
5.2  Identification tests:
5.2.1        Chlorides test:
5.2.1.1  Material and equipment:
5.2.1.1.1        Glassware (according to requirement).
5.2.1.1.2        Dilute nitric acid.
5.2.1.1.3        Purified water.
5.2.1.1.4        0.4ml of Silver nitrate R1.
5.2.1.1.5        Ammonia.
5.2.1.2  Sample:
5.2.1.2.1        Quantity of substance to be examined equivalent to about 2.0mg of chloride.
5.2.1.3  Method:
5.2.1.3.1        Take a test tube add in it 2.0ml of water with the help of pipette.
5.2.1.3.2        Dissolve in 2.0ml of water a quantity of the substance to be equivalent to about 2.0mg of chloride.
5.2.1.3.3        Acidify with dilute nitric acid.
5.2.1.3.4        And add 0.4ml of silver nitrate R1.
5.2.1.3.5        Shake and allow it to stand.
5.2.1.3.6        A curdled, white ppt is formed.
5.2.1.3.7        Centrifuge it in centrifugation machine,.
5.2.1.3.8        The obtained ppt is wash with 3 quantities, each of 1ml, of water.
5.2.1.3.9        Carry out this operation rapidly is subdued light, degrading the fact that the supernatant solution may not become perfectly clear.
5.2.1.3.10    Suspend the precipitate in 2.0ml of water and add 1.5ml of ammonia.
5.2.1.4  Observations:
5.2.1.4.1        The precipitate dissolves easily with the possible exception of a few large particles which dissolves slowly.
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  Ethanol (96%).
5.3.2.2  0.01M hydrochloric acid.
5.3.2.3  0.1M sodium hydroxide.
5.3.2.4  Thymolphthalein solution as an indicator.
5.3.2.5  Purified water.
5.3.3        Sample:
5.3.3.1  0.320g.
5.3.4        Method of analysis:
5.3.4.1  Take a 50.0ml of beaker and 0.320g of sample in it.
5.3.4.2  Add 50.0ml of ethanol (96%) and add 5.0ml of 0.01M hydrochloric acid in it and dissolve by using magnetic stirrer operate.
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 an indicator.
5.3.4.5  Operate potentiometer.
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-1.
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-1.
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 40.39mg of Bambuterol hydrochloride C18H30ClN3O5.
5.3.6        Limit:
5.3.6.1  98.5% to 101.5% (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 / Bambuterol Hydrochloride: 2015, pp. 236-237.
7.2  The British Pharmacopoeia. Vol V., Official Monograph /Qualitative Reactions and Tests: 2015, pp. 266-270.
8.0  ANNEXURES:
Annexure 1: Assay observations and calculations (Potentiometric titration).

Annexure: 1
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
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
v/s
Verses
mV
Millivolts
oC
Degree centigrade
R
Reagent


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