CROTAMITON SOP



CROTAMITON SOP

1.0  OBJECTIVE:
To lay down a procedure of analytical report for the active raw material of the Crotamiton from the Pharmacopoeial specifications.
2.0  SCOPE:
This SOP shall be applicable in Q.C laboratory.
3.0  RESPONSIBILITY:
3.1  Q.C Analysts.
4.0  ACCOUNTABILITY:
4.1  Q.C Manager.
5.0  PROCEDURE:
5.1  Characters:
5.1.1        Appearance:
5.1.1.1  Colourless or pale yellow.
5.1.1.2  Oily liquid.
5.1.2        Solubility:
5.1.2.1  Material and equipment:
5.1.2.1.1        Glassware (test tubes, spatula).
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 2 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        At low temperature it may partly or completely soluble.
5.1.2.4  Observations:
5.1.2.4.1        The sample in test tube 1 containing with water is slightly soluble.
5.1.2.4.2        The sample in test tubes 2 containing with ethanol (96%) is miscible.
5.2  Identification tests:
5.2.1         
5.2.1.1  Material and equipment:
5.2.1.1.1        Glassware (according to requirement).
5.2.1.1.2        UV/Vis spectrophotometer.
5.2.1.2  Sample:
5.2.1.2.1        25.0mg.
5.2.1.3  Test solution:
5.2.1.3.1        Take a beaker of 100.0ml. Take sample 25.0mg dissolve it in cyclohexane small volume of liquid.
5.2.1.3.2        Dilute it to 100.0ml with the same solvent.
5.2.1.3.3        Again dilute 1.0ml of this solution to 10.0ml with cyclohexane.
5.2.1.4  Spectral range:
5.2.1.4.1        220-300nm.
5.2.1.5  Absorption maximum:
5.2.1.5.1        At 242nm.
5.2.1.6  Specific absorbance at the maximum absorption:
5.2.1.6.1        300-330.
5.2.1.7  Method of analysis:
5.2.1.7.1        According to SOP of UV/visible spectrophotometer operate i.e. and observe the absorbance of test solution.
5.2.1.8  Observations:
5.2.1.8.1        Maximum absorption found at 242nm.
5.2.2         
5.2.2.1  Material and equipment:
5.2.2.1.1        Glassware (test tube, spatula).
5.2.2.1.2        3g/L solution of potassium permanganate.
5.2.2.1.3        Purified water.
5.2.2.2  Sample:
5.2.2.2.1        Saturated solution of active ingredient.
5.2.2.3  Method of analysis:
5.2.2.3.1        Take a test tube and add in it 10ml of a saturated solution.
5.2.2.3.2        Add a few drops of 3g/L solution of potassium permanganate.
5.2.2.3.3        Observe the changes.
5.2.2.4  Observations:
5.2.2.4.1        A brown colour is produced.
5.2.2.4.2        A brown ppt is formed on standing.
5.3  Assay:
5.3.1        Apparatus:
5.3.1.1  HPLC apparatus.
5.3.1.2  Glassware (according to the requirement).
5.3.2        Material and reagents:
5.3.2.1  Tetrahydrofuran 8 volume.
5.3.2.2  Cyclohexane 92 volume.
5.3.3        Requirements:
5.3.3.1  Sample:
5.3.3.1.1        50.0mg (sample to be examined).
5.3.3.1.2        50.0mg (Crotamiton CRS) for reference solution.
5.3.3.2  Test solution:
5.3.3.2.1        Test solution (a):
5.3.3.2.1.1  Take 100ml of beaker and dissolve 50.0mg of the substance to be examined in the mobile phase.
5.3.3.2.1.2  And dilute to 100.0ml with the mobile phase.
5.3.3.2.2        Test solution (b):
5.3.3.2.2.1  Take a beaker and dilute 1.0ml of test solution (a) to 20.0ml with the mobile phase.
5.3.3.3  Reference solutions:
5.3.3.3.1        Reference solution (a):
5.3.3.3.1.1  Take 100ml beaker and dissolve 50.0mg of Crotamiton CRS in the mobile phase.
5.3.3.3.1.2  And dilute to 20.0ml with the mobile phase.
5.3.3.3.1.3  Dilute 1.0ml of this solution to 50.0ml with the mobile phase.
5.3.3.4  Column:
5.3.3.4.1        Size:
5.3.3.4.1.1  Length=0.25m,
5.3.3.4.1.2  θ=4mm.
5.3.3.4.2        Stationary phase:
5.3.3.4.2.1  Silica gel for chromatography (5μm).
5.3.3.5  Mobile phase:
5.3.3.5.1        Tetrahydrofuran, cyclohexane (8:92 v/v)
5.3.3.6  Flow rate:
5.3.3.6.1        1.0ml/min.
5.3.3.7  Detection:
5.3.3.7.1        Spectrophotometer at 242nm.
5.3.3.8  Injection:
5.3.3.8.1        20μL of the test solution (b) and reference solution (a).
5.3.3.9  Run time:
5.3.3.9.1        2.5 times the retention time of the (E)-isomer.
5.3.3.10    Relative retention:
5.3.3.10.1    With reference to (E)-isomer: (Z)-isomer=about 0.5.
5.3.4        Method of analysis:
5.3.4.1  Firstly prepare the test solution, reference solution and mobile phase according to the requirements.
5.3.4.2  The solutions must be free from solid particles.
5.3.4.3  Prepare the apparatus.
5.3.4.4  The mobile phase solvent mixtures must be de-aerated prior to use either by boiling or by applying a partial vacuum to the solvent reservoir.
5.3.4.5  Equilibrate the column with the prescribed mobile phase, flow rate and at temperature specified until a suitable baseline is achieved.
5.3.4.6  Test solution of the mixture to be separated is now introduced into the mobile phase with the help of an injector just before entering the separating column.
5.3.4.7  As the eluate leaves the column it enters a detector, where it is continuously monitored at the specified λ.
5.3.4.8  The electrical signal obtained from detector is amplified and routes to recorder which record the developed spectrum.
5.3.4.9  Calculate the percentage content of Crotamiton (C13H17NO) from the sum of the areas of peaks due to (Z) - and (E)-isomers in the spectrum obtained.
5.3.4.10    Calculate the content of the (Z)-isomer, as a percentage of the total content of the (E) - and (Z)-isomers, from the chromatogram obtained with test solution (b).
5.3.5        Observations:
5.3.5.1  Sum of the (E)- and (Z)-isomers:
5.3.5.1.1        96% to 102%.
5.3.5.2  (Z)-isomer:
5.3.5.2.1        15%.
6.0  REVISION LOG:
Revision No.
Effective Date
Reason
00

New SOP

7.0  REFERENCES:
7.1  The British Pharmacopoeia. Vol I., Official Monograph /Crotamiton: 2015, pp. 655-657.
8.0  ANNEXURES:
8.1  Not Applicable.



9.0  ABBREVIATIONS:
Abbreviation
Expanded Form
SOP
Standard operating procedure
&
And
No.
Number 
Ltd.
Limited
Q.C
Quality control
%
Percentage
B.P
British pharmacopoeia
UV
Ultraviolet
mg
Milligram
ml
Milliliter
nm
Nanometer
g/L
Gram per liter
ppt
Precipitate
CRS
Control reference solution
g
Grams
θ
Theta
μm
Micrometer
m
Meter
v/v
Volume by volume
ml/min
Milliliter per minute
μL
Microliter
%
Percentage
λ
lamda
Vol
Volume
QCA
Quality control active ingredient
F
Format


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