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:
Average: _______________
Optical
rotation of blank solution: _______________
Sample solution:
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:
Plot
a graph, volume used v/s millivolts and find out peak of graph i.e. END POINT
of blank titration.
Sample
titration:
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
|
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