DEXLANSOPRAZOLE SOP

DEXLANSOPRAZOLE SOP

1.0  OBJECTIVE:
To lay down a procedure for the active raw material of the Dexlansoprazole 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 brownish 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        Anhydrous ethanol.
5.1.2.1.3        Acetonitrile.
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 Anhydrous ethanol in test tube 2 and observe
5.1.2.3.4        Add Acetonitrile in test tube 3 and observe.
5.1.2.4  Observations:
5.1.2.4.1        The sample in test tube 1 containing with purified water is very practically insoluble.
5.1.2.4.2        The sample in test tube 2 containing with anhydrous ethanol is soluble.
5.1.2.4.3        The sample in test tube 3 containing with Acetonitrile is slightly soluble.
5.2  Identification test:
5.2.1        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        Magnetic stirrer.
5.2.1.1.4        Glassware (1 beaker of 50.0ml, 1 stirrer, 1 spatula).
5.2.1.1.5        15.0ml of dilute hydrochloric acid.
5.2.1.1.6        Purified water.
5.2.1.2  Sample:
5.2.1.2.1        2.25g
5.2.1.3  Method:
5.2.1.3.1        Take a beaker of 50.0ml and add 2.25g of sample in it.
5.2.1.3.2        Dissolve it in 15.0ml of dilute hydrochloric acid by using magnetic stirrer operate according to SOP
5.2.1.3.3        And then dilute it to 50.0mlwith purified water.
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.
5.2.1.4  Observations:
5.2.1.4.1        The optical rotation is +142°+149°.
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  40.0ml of ethanol (96%).
5.3.2.2  0.1M sodium hydroxide.
5.3.2.3  Thymolphthalein solution (as indicator).
5.3.2.4  Purified water.
5.3.3        Sample:
5.3.3.1  0.300g.
5.3.4        Method of analysis:
5.3.4.1  Take a 100.0ml of beaker and take 0.300g of sample in it.
5.3.4.2  And add 40.0ml of ethanol (96%) dissolve it by using magnetic stirrer operate according to SOP.
5.3.4.3  Dilute it to 50.0ml with purified water.
5.3.4.4  Fill the right hand side burette with titrant 0.1M sodium hydroxide.
5.3.4.5  Carry out a Potentiometric titration using thymolphthalein solution (as indicator).
5.3.4.6  Operate potentiometer according to SOP.
5.3.4.7  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-1.
5.3.4.8  Plot a graph, volume used v/s millivolts.
5.3.4.9  Find out the END POINT.
5.3.4.10       Peak of graph indicates END POINT i.e. the point at which maximum millivolts. Note down volume used at that point.
5.3.4.11       Perform blank titration without using sample. Similarly, as sample titration performed. Record observations in annexure-1.
5.3.4.12       Calculate volume used by substance by using formula:
Volume used by substance = Blank titration - Sample titration.
5.3.4.13       Calculate percentage purity of the sample by using formula:
%age purity = volume used by substance x factor x 100
                           Weight of sample
5.3.5        Factor:
5.3.5.1  1ml of 0.1M sodium hydroxide is equivalent to 36.94mg of Dexlansoprazole C16H14F3N3O2S.
5.3.6        Limit:
5.3.6.1  99.0% to 101.0% (dried substance).
6.0  REVISION LOG:
Revision No.
Effective Date
Reason
00

New SOP

7.0  REFERENCES:
7.1  Manufacturer specifications.
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
fQCA
Quality control active ingredient
F
Format
Q.C
Quality control
v/s
Verses
mV
Millivolts
g
Grams
ml
Milliliter
oC
Degree centigrade
mg
Milligram
M
Molar
%
Percentage
R
Reagent
o
Degree (angle)
l
Length
c
Concentration (g/ml)
g/ml
Gram per milliliter
α
Alpha
λ
Lambda

No comments:

Post a Comment