SIMETICONE METHOD OF ANALYSIS SOP


SIMETICONE METHOD OF ANALYSIS SOP


1.0  OBJECTIVE:
To lay down a procedure for the active raw material of the Simeticone 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  Viscous, grayish-white, opalescent liquid.
5.1.2        Solubility:
5.1.2.1  Material and equipment:
5.1.2.1.1        Glassware (7 test tubes, 1 spatula, 1 pipette).
5.1.2.1.2        Anhydrous ethanol.
5.1.2.1.3        Ethyl acetate.
5.1.2.1.4        Methylene chloride.
5.1.2.1.5        Methyl ethyl ketone.
5.1.2.1.6        Toulene.
5.1.2.1.7        Purified water.
5.1.2.1.8        Methanol.
5.1.2.2  Sample:
5.1.2.2.1        Small quantity.
5.1.2.3  Method:
5.1.2.3.1        Take 7 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 Methanol in test tube 3 and observe.
5.1.2.3.5        Add Ethyl acetate in test tube 4 and observe.
5.1.2.3.6        Add Methylene chloride in test tube 5 and observe.
5.1.2.3.7        Add Methyl ethyl ketone in test tube 6 and observe.
5.1.2.3.8        Add Toulene in test tube 7 and observe.
5.1.2.4  Observations:
5.1.2.4.1        The sample in test tube 1 containing with purified water is practically insoluble.
5.1.2.4.2        The sample in test tube 2 containing with anhydrous ethanol is very slightly soluble or practically insoluble.
5.1.2.4.3        The sample in test tube 3 containing with Methanol is practically insoluble.
5.1.2.4.4        The sample in test tube 4, 5, 6 & 7 containing with ethyl acetate, Methylene chloride, Methyl ethyl ketone and toluene is partly miscible.
5.2  Identification tests:
5.2.1         
5.2.1.1  Material and equipment:
5.2.1.1.1        Glassware (2 test tubes, 1 pipette, 1 spatula).
5.2.1.1.2        Analytical weighing balance.
5.2.1.1.3        Burner.
5.2.1.1.4        Water-bath.
5.2.1.1.5        1.0ml of a 1g/L solution of chromotropic acid, sodium salt R in sulfuric acid.
5.2.1.2  Sample:
5.2.1.2.1        0.5g.
5.2.1.3  Method:
5.2.1.3.1        Take test tube A and add in it 0.5g of sample in it.
5.2.1.3.2        Heat it over a small flame until white fumes begin to appear.
5.2.1.3.3        Take test tube B containing 1.0ml of a 1g/L solution of chromotropic acid, sodium salt R in sulfuric acid.
5.2.1.3.4        Invert the test tube A over a test tube B, so that the fumes reach the solution.
5.2.1.3.5        Shake the test tube B for about 10s and eat on water-bath for 5min.
5.2.1.3.6        Observe the changes.
5.2.1.4  Observations:
5.2.1.4.1        The solution is violet.
5.2.2        Silicates test:
5.2.2.1  Material and equipment:
5.2.2.1.1        Glassware (1 spatula, 1 pipette, 1 crucible, 1 copper wire).
5.2.2.1.2        Water-bath.
5.2.2.1.3        10.0mg of sodium fluoride.
5.2.2.1.4        Sulfuric acid.
5.2.2.1.5        Purified water.
5.2.2.2  Sample:
5.2.2.2.1        The residue obtained in the test for silica under assay 5.3.
5.2.2.3  Method:
5.2.2.3.1        Take a lead or a platinum crucible add in it prescribed quantity of the substance, mix it by means of a copper wire with about 10.0mg of sodium fluoride and a few drops of Sulfuric acid to give a thin slurry.
5.2.2.3.2        Cover the crucible with a thin, transparent plate of plastic under which a drop of purified water is suspended and warm it gently on water bath.
5.2.2.3.3        Observe the changes.
5.2.2.4  Observations:
5.2.2.4.1        Within a short time a white ring is rapidly formed around the drop of purified water. (7.1) (7.2)
5.3  Assay:
5.3.1        IR absorption Spectrophotometry:
5.3.1.1  Material and equipment:
5.3.1.1.1        Glassware (according to requirement).
5.3.1.1.2        IR Spectrophotometer.
5.3.1.1.3        Magnetic stirrer.
5.3.1.1.4        2mg/ml of USP Polydimethylsiloxane RS.
5.3.1.1.5        Toluene.
5.3.1.1.6        Dilute hydrochloric acid.
5.3.1.1.7        Anhydrous sodium sulfate.
5.3.1.2  Sample:
5.3.1.2.1        50.0mg.
5.3.1.3  Standard stock solution:
5.3.1.3.1        Take a beaker and prepare standard stock solution according to need 2mg/ml of USP Polydimethylsiloxane RS in toluene.
5.3.1.4  Standard solution:
5.3.1.4.1        Take a round, narrow-mouth, screw-capped 120.0ml of bottle and add 25.0ml of standard stock solution in it.
5.3.1.4.2        Add 50.0ml of dilute hydrochloric acid (2 in 5) in it, close the bottle securely with a cap having an inert liner, and shake for 5min , accurately timed , on a reciprocating shaker at a suitable rate (e.g. about 200 oscillations/min and a stroke of 38±2mm).
5.3.1.4.3        Transfer the mixture to a 125.0ml separator, and remove 5.0ml of the upper organic (toluene) layer to a 15.0ml, screw-capped test tube containing 0.5g of anhydrous sodium sulfate.
5.3.1.4.4        Close the tube with a screw-cap having an inert liner, agitate vigorously, and centrifuge the mixture until a clear supernatant is obtained.
5.3.1.5  Sample stock solution:
5.3.1.5.1        Take a round, narrow-mouth, screw-capped 120.0ml of bottle and add 50.0mg of Simeticone.
5.3.1.5.2        Add 25.0ml of toluene and swirl to disperse by using magnetic stirrer.
5.3.1.6  Sample solution:
5.3.1.6.1        Take a round, narrow-mouth, screw-capped 120.0ml of bottle and add 50.0mg of Simeticone.
5.3.1.6.2        Add 25.0ml of toluene and swirl to disperse by using magnetic stirrer.
5.3.1.6.3        Add 50.0ml of dilute hydrochloric acid (2 in 5) in it, close the bottle securely with a cap having an inert liner, and shake for 5min , accurately timed , on a reciprocating shaker at a suitable rate (e.g. about 200 oscillations/min and a stroke of 38±2mm).
5.3.1.6.4        Transfer the mixture to a 125.0ml separator, and remove 5.0ml of the upper organic (toluene) layer to a 15.0ml, screw-capped test tube containing 0.5g of anhydrous sodium sulfate.
5.3.1.6.5        Close the tube with a screw-cap having an inert liner, agitate vigorously, and centrifuge the mixture until a clear supernatant is obtained.
5.3.1.7  Blank:
5.3.1.7.1        Take a round, narrow-mouth, screw-capped 120.0ml of bottle and add 25.0ml of toluene.
5.3.1.7.2        Add 50.0ml of dilute hydrochloric acid (2 in 5) in it, close the bottle securely with a cap having an inert liner, and shake for 5min , accurately timed , on a reciprocating shaker at a suitable rate (e.g. about 200 oscillations/min and a stroke of 38±2mm).
5.3.1.7.3        Transfer the mixture to a 125.0ml separator, and remove 5.0ml of the upper organic (toluene) layer to a 15.0ml, screw-capped test tube containing 0.5g of anhydrous sodium sulfate.
5.3.1.7.4        Close the tube with a screw-cap having an inert liner, agitate vigorously, and centrifuge the mixture until a clear supernatant is obtained.
5.3.1.8  Instrumental conditions:
5.3.1.8.1        Mode: IR.
5.3.1.8.2        Analytical wavelength: Wavelength of maximum absorbance at about 7.9μm.
5.3.1.8.3        Cell: 0.5mm.
5.3.1.9  Method of analysis:
5.3.1.9.1        Samples: Standard stock solution, Standard solution, Sample stock solution and Sample solution.
5.3.1.9.2        Switch ON the IR spectrophotometer and operate it according to SOP No. BM/QCEO/SOP024-00.
5.3.1.9.3        Determine the absorbance of the samples, using the Blank to set the instrument.
5.3.1.9.4        Calculate the percentage of the Polydimethylsiloxane [-(CH3)2SiO-]n in the portion of Simeticone taken:
Result: (AU/AS) x (CS/CU) x 100
AU = absorbance of the sample solution.
AS = absorbance of the standard solution.
CS = concentration of USP Polydimethylsiloxane RS in the standard stock solution (mg/ml).
CU = concentration of simethicone in the sample stock solution (mg/ml).
5.3.1.10    Acceptance criteria:
5.3.1.10.1    90.5%-99.0%. (7.3)
6.0  REVISION LOG:
Revision No.
Effective Date
Reason
00

New SOP

7.0  REFERENCES:
7.1  The British Pharmacopoeia. Vol II., Official Monograph /Simeticone: 2015, pp. 810-811.
7.2  The British Pharmacopoeia. Vol V., Official Monograph /Qualitative Reactions and Tests: 2015, pp. 266-270.
7.3  USP38NF33 Volume-6 Official Monograph/ Simethicone: 2015, pp.: 5295-5296.
8.0  ANNEXURES:
Annexure 1: Calculations of IR-spectrophotometer

Annexure: 1
Calculations of IR-spectrophotometer
IR-spectrophotometer
Model: _____________________________                             Date: _________________
OBSERVATIONS:
Thickness of cell:

Maxima absorption wavelength

Sample:

Other reagent used:

Blank solution:
No. of obs.
Concentration
(CU)
Wavelength
Absorbance
(AU)








Standard solution:
No. of obs.
Concentration
(CS)
Wavelength
Absorbance
(AS)








Sample solution:
No. of obs.
Concentration
(CU)
Wavelength
Absorbance
(AU)












CALCULATIONS:
Result: (AU/AS) x (CS/CU) x 100









Results: _______________
Remarks: ______________________________________________________________
















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
BP
British Pharmacopoeia
mg
Milligram
ml
Milliliter
M
Molar
g
Grams
s
Seconds
Min
Minute
%
Percentage
R
Reagent
oC
Degree centigrade
IR spectrophotometer
Infrared spectrophotometer
mg/ml
Milligram per milliliter
USP
United states pharmacopoeia
RS
Reference standard
NF
National formulary
μm
Micrometer
mm
Millimeter
g/L
Grams per liter


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