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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