BENZYL BENZOATE SOP


BENZYL BENZOATE SOP

1.0  OBJECTIVE:
To lay down a procedure of analytical report for the active raw material of the Benzyl benzoate 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 almost colourless crystals.
5.1.1.2  Colourless or almost colourless 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        Purified water.
5.1.2.1.3        Ethanol (96%).
5.1.2.1.4        Methylene chloride.
5.1.2.1.5        Fatty oils.
5.1.2.1.6        Essential oils.
5.1.2.2  Sample:
5.1.2.2.1        Small quantity.
5.1.2.3  Method:
5.1.2.3.1        Take 5 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        Add methylene chloride in test tube 3 and observe.
5.1.2.3.5        Add fatty oils in test tube 4 and observe.
5.1.2.3.6        Add essential oils in test tube 5 and observe.
5.1.2.4  Observations:
5.1.2.4.1        The sample in test tube 1 containing with water is practically insoluble.
5.1.2.4.2        The sample in test tubes 2, 3, 4 and 5 containing with ethanol (96%), methylene chloride, fatty oils and essential oils is miscible respectively.
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        Reflux condenser.
5.2.1.1.3        Water-bath.
5.2.1.1.4        Melting point apparatus (beaker, stirrer, thermometer, capillary tube, burner, thread).
5.2.1.1.5        Alcoholic potassium hydroxide.
5.2.1.1.6        Dilute hydrochloric acid.
5.2.1.1.7        Purified water.
5.2.1.2  Sample:
5.2.1.2.1        2.0 g.
5.2.1.3  Method of analysis:
5.2.1.3.1        Set the apparatus of reflux condenser.
5.2.1.3.2        Add 2.0g of sample in conical flask with 25.0ml of alcoholic potassium hydroxide.
5.2.1.3.3        Boil under the reflux condenser for 2 hr.
5.2.1.3.4        Remove the ethanol on water-bath.
5.2.1.3.5        Add 50.0ml of water and distill it.
5.2.1.3.6        Collect about 25.0ml of distillate use it for the test 5.2.2.
5.2.1.3.7        And remaining distillate acidifies with dilute hydrochloric acid in the distillation flask.
5.2.1.3.8        A white ppt is formed.
5.2.1.3.9        Wash with water.
5.2.1.3.10    Dried in vacuo.
5.2.1.3.11    Determine its melting point.
5.2.1.3.12    Melting point determination method:
5.2.1.3.12.1    Firstly set the apparatus.
5.2.1.3.12.2    Fill 100ml beaker with water and place wire gauze on tripod stand, put beaker on it.
5.2.1.3.12.3    Heat up the capillary tube on burner from center such that it divides into two by pulling the capillary tube from both sides in opposite directions.
5.2.1.3.12.4    Introduce a sufficient quantity into a capillary tube to give a compact column 4mm to 6mm in height.
5.2.1.3.12.5    Tie up the capillary tube near the thermometer bulb with the help of thread.
5.2.1.3.12.6    And hang the thermometer on stand such that the capillary tube is not fully immersed in water. The immersion mark of which is at the level of the surface of the liquid.
5.2.1.3.12.7    Allow the burner to heat up the liquid in beaker.
5.2.1.3.12.8    Observe it closely.
5.2.1.3.12.9    Record the temperature at which the last particle passes into the liquid phase.
5.2.1.4  Observations:
5.2.1.4.1        The residue melts at 121oC to 124oC.
5.2.2         
5.2.2.1  Material and equipment:
5.2.2.1.1        Glassware (according to requirement).
5.2.2.1.2        Reflux condenser.
5.2.2.1.3        Water-bath.
5.2.2.1.4        Filter paper.
5.2.2.1.5        Melting point apparatus (beaker, stirrer, thermometer, capillary tube, burner, thread).
5.2.2.1.6        Potassium permanganate.
5.2.2.1.7        Dilute sodium hydroxide.
5.2.2.1.8        Dilute hydrochloric acid.
5.2.2.1.9        Purified water.
5.2.2.2  Sample:
5.2.2.2.1        Distillate 25.0ml obtained from the 5.2.1.
5.2.2.3  Method of analysis:
5.2.2.3.1        Set the apparatus of reflux condenser.
5.2.2.3.2        To the distillate obtained from 5.2.1 add 2.5g of potassium permanganate and 5.0ml of dilute sodium hydroxide solution.
5.2.2.3.3        Boil under the reflux condenser for 15 min.
5.2.2.3.4        Cool it.
5.2.2.3.5        Filter it.
5.2.2.3.6        Acidify the filtrate with dilute hydrochloric acid.
5.2.2.3.7        A white ppt is formed.
5.2.2.3.8        Wash with water.
5.2.2.3.9        Dried in vacuo.
5.2.2.3.10    Determine its melting point.
5.2.2.3.11    Melting point determination method:
5.2.2.3.11.1    Firstly set the apparatus.
5.2.2.3.11.2    Fill 100ml beaker with water and place wire gauze on tripod stand, put beaker on it.
5.2.2.3.11.3    Heat up the capillary tube on burner from center such that it divides into two by pulling the capillary tube from both sides in opposite directions.
5.2.2.3.11.4    Introduce a sufficient quantity into a capillary tube to give a compact column 4mm to 6mm in height.
5.2.2.3.11.5    Tie up the capillary tube near the thermometer bulb with the help of thread.
5.2.2.3.11.6    And hang the thermometer on stand such that the capillary tube is not fully immersed in water. The immersion mark of which is at the level of the surface of the liquid.
5.2.2.3.11.7    Allow the burner to heat up the liquid in beaker.
5.2.2.3.11.8    Observe it closely.
5.2.2.3.11.9    Record the temperature at which the last particle passes into the liquid phase.
5.2.2.4  Observations:
5.2.2.4.1        The residue melts at 121oC to 124oC.
5.3  Assay:
5.3.1        Apparatus:
5.3.1.1  Glassware (according to requirement).
5.3.1.2  Reflux condenser.
5.3.1.3  Titration apparatus.
5.3.2        Material and reagents:
5.3.2.1  0.5M alcoholic potassium hydroxide.
5.3.2.2  0.5M hydrochloric acid.
5.3.2.3  Phenolphthalein (as an indicator).
5.3.3        Sample:
5.3.3.1  2.0g.
5.3.4        Method of analysis:
5.3.4.1  Set the apparatus of reflux condenser.
5.3.4.2  Add 2.0g of sample in conical flask with 50.0ml of alcoholic potassium hydroxide.
5.3.4.3  Boil gently under the reflux condenser for 1hr.
5.3.4.4  Set titration apparatus.
5.3.4.5  Titrate the above hot solution with 0.5M hydrochloric acid using 1ml of phenolphthalein solution (as indicator).
5.3.4.6  Carry out a blank determination.
5.3.5        Factor:
5.3.5.1  1ml of 0.5M alcoholic potassium hydroxide is equivalent to 106.1mg of C14H12O2.
6.0  REVISION LOG:
Revision No.
Effective Date
Reason
00

New SOP

7.0  REFERENCES:
7.1  The British Pharmacopoeia. Vol I., Official Monograph /Benzyl benzoate: 2015, pp. 268.
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
g
Grams
ml
Milliliter
hr
Hour
ppt
Precipitate
mm
Millimeter
oC
Degree centigrade
min
Minutes
M
Molar
mg
Milligram
Vol
Volume
QCA
Quality control active ingredient
F
Format



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