SODIUM PICOSULFATE METHOD OF ANALYSIS SOP

SODIUM PICOSULFATE METHOD OF ANALYSIS SOP

1.0  OBJECTIVE:

To lay down a procedure for the active raw material of the Sodium Picosulfate 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  Crystalline powder.

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        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 a test tube 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 1 and observe.

5.1.2.4  Observations:

5.1.2.4.1        The sample in test tube 1 containing with purified water is freely soluble.

5.1.2.4.2        The sample in test tube 1 containing with Ethanol (96) is 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  2.5g.

5.2.3        Preparation of solution S:

5.2.3.1  Take a beaker of 50.0ml and add sample 2.5g in it.

5.2.3.2  Add in it sufficient quantity of carbon-dioxide free water prepared from distilled water.

5.2.3.3  Dilute it to 50.0ml with the same solvent.

5.3  Identification tests:

5.3.1         

5.3.1.1  Material and equipment:

5.3.1.1.1        Glassware (1 test tube, 1 spatula, 1 pipette).

5.3.1.1.2        Burner.

5.3.1.1.3        1.0ml of dilute hydrochloric acid.

5.3.1.1.4        1.0ml of barium chloride solution.

5.3.1.2  Sample:

5.3.1.2.1        5.0ml of solution S.

5.3.1.3  Method:

5.3.1.3.1        Take a beaker and add 5.0ml of solution S in it.

5.3.1.3.2        And add 1.0ml of dilute hydrochloric acid.

5.3.1.3.3        Heat it on burner till boiling.

5.3.1.3.4        Add 1.0ml of barium chloride solution.

5.3.1.3.5        Observe the changes.

5.3.1.4  Observations:

5.3.1.4.1        A white ppt is formed.

5.3.2         

5.3.2.1  Material and equipment:

5.3.2.1.1        Glassware (1 test tube, 1 spatula, 1 pipette).

5.3.2.1.2        Analytical weighing balance.

5.3.2.1.3        3.0ml of sulfuric acid.

5.3.2.1.4        0.1ml of potassium dichromate solution R1.

5.3.2.2  Sample:

5.3.2.2.1        10.0mg.

5.3.2.3  Method:

5.3.2.3.1        Take a test tube and add in it 10.0mg of sample.

5.3.2.3.2        Add 3.0ml of sulfuric acid and 0.1ml of potassium dichromate solution R1

5.3.2.3.3        Observe the changes.

5.3.2.4  Observations:

5.3.2.4.1        A violet colour develops.

5.3.3        Sodium test:

5.3.3.1  Material and equipment:

5.3.3.1.1        Glassware (test tube, spatula, beaker, glass rod).

5.3.3.1.2        Analytical weighing balance.

5.3.3.1.3        Burner.

5.3.3.1.4        2.0ml of 150g/L solution of potassium carbonate.

5.3.3.1.5        4.0ml of potassium pyroantimonate solution.

5.3.3.1.6        Iced water.

5.3.3.1.7        Purified water.

5.3.3.2  Sample:

5.3.3.2.1        2.0ml of solution S.

5.3.3.3  Method:

5.3.3.3.1        Take a test tube and add 2.0ml of solution S.

5.3.3.3.2        Add 2.0ml of 150g/L solution of potassium carbonate and heat it to boiling on burner.

5.3.3.3.3        Observe the changes.

5.3.3.3.4        No ppt is formed.

5.3.3.3.5        Add 4.0ml of potassium pyroantimonate solution again heat it to boiling on burner.

5.3.3.3.6        And then take a beaker of filled with iced water, put test tube in it and allow it to cool.

5.3.3.3.7        If necessary rub the inside of the test tube with a glass rod.

5.3.3.3.8        Observe the changes.

5.3.3.4  Observations:

5.3.3.4.1        A dense white 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  80.0ml of methanol.

5.4.2.2  0.1M Perchloric acid.

5.4.2.3  Crystal violet solution.

5.4.3        Sample:

5.4.3.1  0.4g.

5.4.4        Method of analysis:

5.4.4.1  Take a 100.0ml of beaker and take 0.4g of sample in it.

5.4.4.2  Add 80.0ml of methanol in it and dissolve by using magnetic stirrer i.e. SOP

5.4.4.3  Fill the right hand side burette with titrant 0.1M Perchloric acid.

5.4.4.4  Carry out a Potentiometric titration using crystal violet solution as an indicator.

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-1.

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-1.

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 Perchloric acid is equivalent to 48.14mg of Sodium Picosulfate C₁₈H₁₃NNa₂O₈S₂.

5.4.6        Limit:

5.4.6.1  98.5% to 100.5% (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 / Sodium Picosulfate: 2015, pp. 860-861.

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
QCA	Quality control active ingredient
F	Format
Q.C	Quality control
Vol	Volume
mg	Milligram
ml	Milliliter
ppt	Precipitate
M	Molar
g	Grams
%	Percentage
v/s	Verses
mV	Millivolts
R	Reagent
BP	British Pharmacopoeia