SODIUM SESQUIHYDRATE SOP

1.0  OBJECTIVE:
To lay down a procedure of analytical report for the active raw material of the Pantoprazole sodium sesquihydrate from the Pharmacopoeial specifications.
2.0  SCOPE:
This SOP shall be applicable in Q.C laboratory.
3.0  RESPONSIBILITY:
3.1  Q.C Pharmacist.
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 powder.
5.1.2        Solubility:
5.1.2.1  Material and equipment:
5.1.2.1.1        Glassware (3 test tubes, 1 spatula).
5.1.2.1.2        Ethanol (96%).
5.1.2.1.3        Hexane.
5.1.2.1.4        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 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 hexane 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%) are freely soluble.
5.1.2.4.2        The sample in test tube 3 containing with hexane is practically insoluble.
5.2  Identification tests:
5.2.1        Sodium test:
5.2.1.1  Material and equipment:
5.2.1.1.1        Glassware (1 crucible, 1 beaker, 2 test tubes, 1 glass rod, 1 funnel).
5.2.1.1.2        Bunsen burner.
5.2.1.1.3        2.0ml of 150g/L solution of potassium carbonate.
5.2.1.1.4        4.0ml of potassium pyroantimonate solution.
5.2.1.1.5        Ice water.
5.2.1.1.6        Purified water (q.s)
5.2.1.2  Sample:
5.2.1.2.1        0.1g.
5.2.1.3  Method:
5.2.1.3.1        Take a test tube and add 0.1g of sample in it.
5.2.1.3.2        Dissolve it with 2.0ml of purified water.
5.2.1.3.3        Add 2.0ml of the 150g/L solution of potassium carbonate
5.2.1.3.4        Heat it on Bunsen burner till boiling.
5.2.1.3.5        No ppt is formed.
5.2.1.3.6        Add 4.0ml of potassium pyroantimonate solution heat on burner till boiling.
5.2.1.3.7        Take a beaker of ice water. And cool the test tube into it, if necessary rub inside of the test tube with a glass rod.
5.2.1.3.8        Observe the changes.
5.2.1.4  Observations:
5.2.1.4.1        A dense white precipitate is formed.
5.3  Optical rotation:
5.3.1        Material and equipment:
5.3.1.1  Polarimeter.
5.3.1.2  Analytical weighing balance.
5.3.1.3  pH meter.
5.3.1.4  Glassware (1 beaker of 50.0ml, 1 stirrer, 1 spatula).
5.3.1.5  8g/L solution of sodium hydroxide.
5.3.1.6  Purified water (q.s).
5.3.2        Sample:
5.3.2.1  0.2g of sample.
5.3.3        Method:
5.3.3.1  Test solution:
5.3.3.1.1        Take a beaker of 50.0ml and dissolve 0.2g of sample in 10.0ml of purified water.
5.3.3.1.2        Adjust pH 11.5-12.0 with 8g/L solution of sodium hydroxide by using pH meter. Operate pH meter according to SOP
5.3.3.1.3        Dilute it to 20.0ml with purified water.
5.3.3.2  Firstly clean the Polarimeter with clean dry cloth, according to SOP
5.3.3.3  Operate the Polarimeter according to SOP.
5.3.3.4  Fill the Polarimeter tube with blank solution and determine the observed optical rotation.
5.3.3.5  Similarly, fill the Polarimeter tube with sample solution and determine the observed optical rotation.
5.3.3.6  Note down the values in annexure-1.
5.3.3.7  Calculate the optical rotation of substance by subtracting sample solution observed optical rotation from the blank optical rotation.
Optical rotation of substance = Blank solution - Sample solution.
5.3.4        Observations:
5.3.4.1  -0.4o to +0.4o.
5.4  Assay:
5.4.1        Apparatus:
5.4.1.1  Glassware (according to requirement).
5.4.1.2  Potentiometer.
5.4.2        Material and reagents:
5.4.2.1  80.0ml of anhydrous acetic acid.
5.4.2.2  5.0ml of acetic acid.
5.4.2.3  0.1M Perchloric acid.
5.4.2.4  Crystal violet solution (as indicator).
5.4.3        Sample:
5.4.3.1  0.200g.
5.4.4        Method of analysis:
5.4.4.1  Take a 100.0ml of beaker and add 0.200g of sample in it.
5.4.4.2  Add 80.0ml of anhydrous acetic acid in it and dissolve by using magnetic stirrer i.e. SOP.
5.4.4.3  Add 5.0ml of acetic acid and dissolve by using magnetic stirrer for at least 10min.
5.4.4.4  Fill the right hand side burette with titrant 0.1M Perchloric acid.
5.4.4.5  Carry out a Potentiometric titration using crystal violet solution as an indicator.
5.4.4.6  Operate potentiometer according to SOP.
5.4.4.7  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.
5.4.4.8  Plot a graph, volume used v/s millivolts.
5.4.4.9  Find out the END POINT.
5.4.4.10    Peak of graph indicates END POINT i.e. the point at which maximum millivolts. Note down volume used at that point.
5.4.4.11    Perform blank titration without using sample. Similarly, as sample titration performed. Record observations in annexure-2.
5.4.4.12    Calculate volume used by substance by using formula:
Volume used by substance = Blank titration - Sample titration.
5.4.4.13    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 Perchloric acid is equivalent to 20.27mg of Pantoprazole sodium sesquihydrate C16H14F2N3NaO4S.
5.4.6        Limit:
5.4.6.1  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 II., Official Monograph / Pantoprazole sodium sesquihydrate: 2015, pp. 494-495.
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.









                                                                      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
Q.C
Quality control
B.P
British pharmacopoeia
Vol
Volume
QCA
Quality control active ingredient
F
Format
q.s
Quantity sufficient
M
Molar
g
Grams
v/s
Verses
%
Percentage
mV
Millivolts
oC
Degree centigrade
ml
Milliliter
ppt
Precipitate
o
Degree (angle)
l
Length
g
Grams
c
Concentration (g/ml)
Min
Minutes
mg
Milligram
α
Alpha
λ
Lambda
T
Temperature
Sr.#
Serial number
g/L
Grams per liter


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