OMEPRAZOLE SODIUM SOP


1.0  OBJECTIVE:
To lay down a procedure for the active raw material of the Omeprazole sodium 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  Hygroscopic powder.
5.1.2        Solubility:
5.1.2.1  Material and equipment:
5.1.2.1.1        Glassware (4 test tubes, 1 spatula).
5.1.2.1.2        Ethanol (96%).
5.1.2.1.3        Purified water.
5.1.2.1.4        Propylene glycol.
5.1.2.1.5        Methylene chloride.
5.1.2.2  Sample:
5.1.2.2.1        Small quantity.
5.1.2.3  Method:
5.1.2.3.1        Take 4 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 Propylene glycol in test tube 3 and observe.
5.1.2.3.5        Add Methylene chloride in test tube 4 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 freely soluble.
5.1.2.4.2        The sample in test tube 3 containing with Propylene glycol is soluble.
5.1.2.4.3        The sample in test tube 4 containing with Methylene chloride is very slightly soluble.
5.2  Solution S:
5.2.1        Material and equipment:
5.2.1.1  Glassware (1 50.0ml of beaker, 1 spatula, 1 glass rod, 1 pipette).
5.2.1.2  Analytical weighing balance.
5.2.1.3  Magnetic stirrer.
5.2.1.4  Carbon dioxide free water.
5.2.2        Sample:
5.2.2.1  0.50g.
5.2.3        Preparation of solution S:
5.2.3.1  Take a beaker of 50.0ml and add sample 0.50g in it.
5.2.3.2  Add in it sufficient quantity of Carbon dioxide free water and mix by using magnetic stirrer i.e. SOP
5.2.3.3  Dilute it to 25.0ml with the same solvent.
5.3  Identification tests:
5.3.1        Optical rotation:
5.3.1.1  Material and equipment:
5.3.1.1.1        Polarimeter.
5.3.1.1.2        Analytical weighing balance.
5.3.1.1.3        Magnetic stirrer.
5.3.1.1.4        Glassware (1 beaker of 50.0ml, 1 stirrer, 1 spatula).
5.3.1.1.5        Purified water.
5.3.1.2  Sample:
5.3.1.2.1        Solution S.
5.3.1.3  Method:
5.3.1.3.1        Take a beaker of 50.0ml and add Solution S in it.
5.3.1.3.2        Firstly clean the Polarimeter with clean dry cloth, according to SOP.
5.3.1.3.3        Operate the Polarimeter according to SOP.
5.3.1.3.4        Fill the Polarimeter tube with blank solution and determine the observed optical rotation.
5.3.1.3.5        Similarly, fill the Polarimeter tube with sample solution and determine the observed optical rotation.
5.3.1.3.6        Note down the values in annexure-1.
5.3.1.4  Observations:
5.3.1.4.1        -0.10o to +0.10o.
5.3.2        Determination of sodium salts:
5.3.2.1  Material and equipment:
5.3.2.1.1        Glassware (according to requirement).
5.3.2.1.2        Analytical weighing balance.
5.3.2.1.3        Burner.
5.3.2.1.4        Ice-water.
5.3.2.1.5        1.5ml of methoxyphenylacetic reagent R.
5.3.2.1.6        1.0ml of dilute ammonia R1.
5.3.2.1.7        1.0ml of ammonium carbonate solution R.
5.3.2.1.8        Purified water
5.3.2.2  Sample:
5.3.2.2.1        1.0g of sample.
5.3.2.3  Method:
5.3.2.3.1        Ignite 1.0g of sample in a china dish. And cool it.
5.3.2.3.2        Add 1.0ml of purified water to the above obtained residue.
5.3.2.3.3        Neutralize it with hydrochloric acid.
5.3.2.3.4        Filter it by using filtration apparatus.
5.3.2.3.5        The obtained filtrate is diluted to 4.0ml with purified water.
5.3.2.3.6        Take 0.1ml of the above solution.
5.3.2.3.7        Add 1.5ml of methoxyphenylacetic reagent R.
5.3.2.3.8        Cool in ice-water for 30min.
5.3.2.3.9        Observe the changes.
5.3.2.3.10    A voluminous, white, crystalline ppt is formed.
5.3.2.3.11    Place in water at 20oC and stir for 5min.
5.3.2.3.12    The ppt does not disappear.
5.3.2.3.13    Add 1.0ml of dilute ammonia R1.
5.3.2.3.14    The ppt dissolves completely.
5.3.2.3.15    Add 1.0ml of ammonium carbonate solution R.
5.3.2.3.16    Observe the changes.
5.3.2.4  Observations:
5.3.2.4.1        No ppt is formed.
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 purified water.
5.4.2.2  0.1M hydrochloric acid.
5.4.3        Sample:
5.4.3.1  0.300g.
5.4.4        Method of analysis:
5.4.4.1  Take a 100.0ml of beaker and take 0.300g of sample in it.
5.4.4.2  Add 50.0ml of purified water in it dissolve it by using magnetic stirrer i.e..
5.4.4.3  Fill the right hand side burette with titrant 0.1M hydrochloric acid.
5.4.4.4  Carry out a Potentiometric titration.
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 0.1M hydrochloric acid corresponds to 36.74mg of Omeprazole sodium C17H18N3NaO3S.
5.4.6        Limit:
5.4.6.1  98.0% 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 II., Official Monograph / Omeprazole: 2015, pp. 442-444.
8.0  ANNEXURES:
Annexure 1: Optical rotation observations and calculations
Annexure 2: Assay observations and calculations (Potentiometric titration).












Annexure: 1
Optical rotation observations and calculations
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
QCA
Quality control active ingredient
F
Format
Q.C
Quality control
Vol
Volume
v/s
Verses
mV
Millivolts
g
Grams
ml
Milliliter
Min
Minutes
oC
Degree centigrade
mg
Milligram
M
Molar
%
Percentage
R
Reagent
o
Degree (angle)
l
Length
g
Grams
c
Concentration (g/ml)
g/ml
Gram per milliliter
α
Alpha
λ
Lambda
T
Temperature


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