GUAIFENESIN SOP


1.0  OBJECTIVE:
To lay down a procedure for the active raw material of the Guaifenesin 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 almost white crystalline powder.
5.1.2        Solubility:
5.1.2.1  Material and equipment:
5.1.2.1.1        Glassware (2 test tubes, 1 spatula).
5.1.2.1.2        Alcohol.
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 alcohol in test tube 2 and observe.
5.1.2.4  Observations:
5.1.2.4.1        The sample in test tube 1 containing with purified water is sparingly soluble.
5.1.2.4.2        The sample in test tube 2 containing with alcohol is soluble.
5.2  Identification tests:
5.2.1        Melting point determination:
5.2.1.1  Material and equipment:
5.2.1.1.1        Glassware (according to requirement).
5.2.1.1.2        Melting point apparatus.
5.2.1.1.3        Capillary tubes.
5.2.1.1.4        Purified water.
5.2.1.2  Sample:
5.2.1.2.1        Sufficient quantity of sample.
5.2.1.3  Method:
5.2.1.3.1        Introduce the sufficient quantity of sample into a capillary tube.
5.2.1.3.2        Set the apparatus and immerse the capillary tube into the apparatus such that the closed end is near the center of the bulb of thermometer.
5.2.1.3.3        Switch on the melting point apparatus.
5.2.1.3.4        Operate the melting point apparatus according to the SOP.
5.2.1.3.5        Raise the temperature of the apparatus.
5.2.1.3.6        Record the temperature at which the last particle passes into the liquid phase.
5.2.1.3.7        Record measurements in annexure-1.
5.2.1.4  Observations:
5.2.1.4.1        The melting point is 79oC-83oC.
5.3  Loss on drying:
5.3.1.1  Material and equipment:
5.3.1.1.1        Glassware (according to requirement).
5.3.1.1.2        Desiccator.
5.3.1.1.3        Diphosphorous pentaoxide.
5.3.1.1.4        Analytical weighing balance.
5.3.1.1.5        Spatula.
5.3.1.2  Sample:
5.3.1.2.1        1.0g.
5.3.1.3  Method:
5.3.1.3.1        Weigh 1g of the test sample.
5.3.1.3.2        Set the desiccator apparatus with desiccant.
5.3.1.3.3        Place the sample into the china dish or petri dish.
5.3.1.3.4        Set the temperature 60oC and at 1.5kPa to 2.5kPa pressure for at least 3h.
5.3.1.3.5        And wait till the sample loses its moisture.
5.3.1.3.6        After 3h weigh the sample again by using analytical weighing balance i.e. the final weight.
5.3.1.3.7        Note down readings on given Annexure-2.
5.3.1.4  Observations:
5.3.1.4.1        Maximum 0.1%.
5.4  Assay:
5.4.1        Apparatus:
5.4.1.1  Glassware (according to requirement).
5.4.1.2  Titration apparatus.
5.4.1.3  Reflux-condenser apparatus.
5.4.1.4  Water-bath.
5.4.2        Material and reagents:
5.4.2.1  Acetic anhydride.
5.4.2.2  Pyridine.
5.4.2.3  0.25ml of phenolphthalein solution R (as indicator).
5.4.2.4  1.0M sodium hydroxide.
5.4.2.5  Purified water.
5.4.3        Sample:
5.4.3.1  0.5g.
5.4.4        Method of analysis:
5.4.4.1  Sample titration:
5.4.4.1.1        Take a beaker of 50.0ml and add 0.5g (m g) of sample in it.
5.4.4.1.2        Add 10.0ml of a freshly prepared mixture of 1 volume of acetic anhydride and 7 volumes of pyridine.
5.4.4.1.3        Set the reflux condenser apparatus.
5.4.4.1.4        Boil under a reflux condenser for 45min.
5.4.4.1.5        Cool it and add 25.0ml of purified water.
5.4.4.1.6        Take a titration flask and add sample solution approximate 10.0ml.
5.4.4.1.7        Set titration apparatus.
5.4.4.1.8        Use 0.25ml of phenolphthalein solution as indicator.
5.4.4.1.9        Titrate with 1.0M sodium hydroxide (n1 ml).
5.4.4.1.10    Note down the volume used as shown in Annexure-3.
5.4.4.1.11    Take at least 3 readings and take average of it.
5.4.4.2  Blank titration:
5.4.4.2.1        Take a beaker of 50.0ml and add 10.0ml of a freshly prepared mixture of 1 volume of acetic anhydride and 7 volumes of pyridine.
5.4.4.2.2        Set the reflux condenser apparatus.
5.4.4.2.3        Boil under a reflux condenser for 45min.
5.4.4.2.4        Cool it and add 25.0ml of purified water.
5.4.4.2.5        Take a titration flask and add sample solution approximate 10.0ml.
5.4.4.2.6        Set titration apparatus.
5.4.4.2.7        Use 0.25ml of phenolphthalein solution as indicator.
5.4.4.2.8        Titrate with 1.0M sodium hydroxide (n2 ml).
5.4.4.2.9        Note down the volume used as shown in Annexure-3.
5.4.4.2.10    Take at least 3 readings and take average of it.
5.4.4.3  Calculate percentage content of Guaifenesin C10H14O4 from the expression:
%age content of Guaifenesin = 19.82 (n2-n1)
      2m
5.4.5        Limit:
5.4.5.1  98.0% to 102.0% (dried substance).

6.0  REVISION LOG:
Revision No.
Effective Date
Reason
00

New SOP

7.0  REFERENCES:
7.1  The British Pharmacopoeia. Vol I., Official Monograph / Guaifenesin: 2015, pp. 1115-1116.
8.0  ANNEXURES:
Annexure 1: Observations of Melting point apparatus.
Annexure 2: Observations of percentage loss of drying.
Annexure 3: Observations and calculations of assay.

Annexure: 1
Observations of Melting point apparatus
Sample = _____________
Time period = _____________
Sr.#
Initial (Ti)
(oC)
Final (Tf)
(oC)
Tf - Ti
(oC)












Average: _____________

Result: _________________

Remarks: _______________________________________________________________





Annexure: 2
Observations of percentage loss of drying
Percentage loss of drying
Apparatus: ____________________
Temperature: __________________
Pressure: _____________________
Weight of Sample = _____________
Time period = _____________
Sr.#
Time (min)
Weight of sample (g)
% Loss of Moisture
Initial weight
Final weight















Average % Loss of Moisture: _____________

% Loss of Moisture:


Remarks: ____________________________________________________________



Annexure: 3
Observations and calculations of assay
Indicator: ___________________
Weight of sample: ____________                                               
Titrant: _____________________
Sample titration
Sr.#
Initial volume (vi)
(ml)
Final volume (vf)
(ml)
vf-vi
(ml)
1.



2.



3.



Average volume: _________________
Blank titration
Sr.#
Initial volume (vi)
(ml)
Final volume (vf)
(ml)
vf-vi
(ml)
1.



2.



3.



Average volume: _________________
Calculations:
Volume used by substance = Blank titration - Sample titration.

%age content of Guaifenesin = 19.82 (n2-n1)
  2m

Result: ____________________________________________________________________



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
%
Percentage
g
Grams
ml
Milliliter
oC
Degree centigrade
mg
Milligram
g
Grams
M
Molar
vi
Initial volume
vf
Final volume
Ti
Initial temperature
Tf
Final temperature


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