EPHEDRINE SOP

1.0  OBJECTIVE:
To lay down a procedure for the active raw material of the Ephedrine 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.
5.1.1.2  Crystalline powder or colorless crystals.
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        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 anhydrous ethanol 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 soluble.
5.1.2.4.2        The sample in test tube 2 containing with anhydrous ethanol is very soluble.
5.2  Identification tests:
5.2.1        Specific optical rotation:
5.2.1.1  Material and equipment:
5.2.1.1.1        Polarimeter.
5.2.1.1.2        Analytical weighing balance.
5.2.1.1.3        Magnetic stirrer.
5.2.1.1.4        Glassware (1 beaker of 50.0ml, 1 stirrer, 1 spatula).
5.2.1.1.5        15.0ml of dilute hydrochloric acid.
5.2.1.1.6        Purified water.
5.2.1.2  Sample:
5.2.1.2.1        2.25g
5.2.1.3  Method:
5.2.1.3.1        Take a beaker of 50.0ml and add 2.25g of sample in it.
5.2.1.3.2        Dissolve it in 15.0ml of dilute hydrochloric acid by using magnetic stirrer operate according to SOP No. BM/QCEO/SOP007-00.
5.2.1.3.3        And then dilute it to 50.0mlwith purified water.
5.2.1.3.4        Firstly clean the Polarimeter with clean dry cloth, according to SOP No. BM/QCEC/SOP031-00.
5.2.1.3.5        Operate the Polarimeter according to SOP No. BM/QCEO/SOP030-00.
5.2.1.3.6        Fill the Polarimeter tube with blank solution and determine the observed optical rotation.
5.2.1.3.7        Similarly, fill the Polarimeter tube with sample solution and determine the observed optical rotation.
5.2.1.3.8        Note down the values in annexure-1.
5.2.1.3.9        Calculate the specific optical rotation with reference to anhydrous substance by using formula:
[α]λ T = α/lc
5.2.1.4  Observations:
5.2.1.4.1        The specific optical rotation is -41 to -43.
5.2.2         
5.2.2.1  Material and equipment:
5.2.2.1.1        Glassware (1 test tube, 1 pipette).
5.2.2.1.2        Analytical weighing balance.
5.2.2.1.3        0.2ml of strong sodium hydroxide solution.
5.2.2.1.4        0.2ml of copper sulfate solution.
5.2.2.1.5        2.0ml of ether.
5.2.2.1.6        1.0ml of purified water.
5.2.2.2  Sample:
5.2.2.2.1        10.0mg.
5.2.2.3  Method:
5.2.2.3.1        Take a test tube and add 10.0mg of sample in it with 1.0ml of purified water, dissolve it.
5.2.2.3.2        Add 0.2ml of strong sodium hydroxide solution and 0.2ml of copper sulfate solution
5.2.2.3.3        Observe the changes.
5.2.2.3.4        A violet colour is produced.
5.2.2.3.5        Add 2.0ml of ether and shake it.
5.2.2.3.6        Observe the changes.
5.2.2.4  Observations:
5.2.2.4.1        The ether layer is purple but, the aqueous layer will be blue.
5.3  Assay:
5.3.1        Apparatus:
5.3.1.1  Glassware (according to requirement).
5.3.1.2  Titration apparatus.
5.3.2        Material and reagents:
5.3.2.1  5.0ml of Alcohol.
5.3.2.2  20.0ml of 0.1M hydrochloric acid.
5.3.2.3  0.05ml of methyl orange red (as indicator).
5.3.2.4  0.1M sodium hydroxide.
5.3.3        Sample:
5.3.3.1  0.2g.
5.3.4        Method of analysis:
5.3.4.1  Sample titration:
5.3.4.1.1        Take a flask and take in it 0.2g of sample.
5.3.4.1.2        Dissolve it in 5.0ml of Alcohol by using glass rod.
5.3.4.1.3        Add 20.0ml of 0.1M hydrochloric acid.
5.3.4.1.4        Set titration apparatus.
5.3.4.1.5        Use 0.05ml of methyl orange red, as indicator.
5.3.4.1.6        Titrate with 0.1M sodium hydroxide, until a yellow colour is obtained.
5.3.4.1.7        Note down the volume used as shown in Annexure-2.
5.3.4.1.8        Take 3 readings at least and take average.
5.3.4.2  Blank titration:
5.3.4.2.1        Take a flask and take in it 5.0ml of Alcohol.
5.3.4.2.2        Add 20.0ml of 0.1M hydrochloric acid.
5.3.4.2.3        Set titration apparatus.
5.3.4.2.4        Use 0.05ml of methyl orange red, as indicator.
5.3.4.2.5        Titrate with 0.1M sodium hydroxide, until a yellow colour is obtained.
5.3.4.2.6        Note down the volume used as shown in Annexure-2.
5.3.4.2.7        Take 3 readings at least and take average.
5.3.4.3  Calculate percentage purity.
5.3.4.4  Calculations:
5.3.4.4.1        After taking average volume of both blank titration and sample titration. Calculate the volume used by the examined substance by using formula:
Volume used by substance = Blank titration - Sample titration.
5.3.4.4.2        For percentage purity use formula:
%age purity = volume used by substance x factor x 100
                                                                              Weight of sample
5.3.4.4.3        Put values and calculate %age purity.
5.3.5        Factor:
5.3.5.1  1ml of 0.1M hydrochloric acid is equivalent to 16.52mg of ephedrine, C10H15NO2.
5.3.6        Limit:
5.3.6.1  99.0% to 101.0% (anhydrous 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 /Ephedrine: 2015, pp. 848-849.
8.0  ANNEXURES:
Annexure 1: Specific optical rotation observations and calculations.
Annexure 2: Observations and calculations of assay.















Annexure: 1
Specific optical rotation observations and calculations
Specific optical rotation
Instrument: ___________________                                              Date: _______________
Model: _______________________        Length of Polarimeter tube: ________________
Sample: ________________________________g.
Solvent: ________________________________ml.
Concentration of sample solution: ____________g/ml.
Blank solution:
Sr.#
Blank solution
Temperature
Optical rotation
(α)












                                                                                                 Average: _______________
Optical rotation of blank solution: _______________
Sample solution:
Sr.#
Sample solution
Temperature
Optical rotation
(α)












                                                                                                 Average: _______________
Optical rotation of sample solution: ______________
Optical rotation of substance = Blank solution - Sample solution.



Specific optical rotation of sample solution by using formula:
[α]λ T = α/lc






                                                                      Result: ________________
Remarks: ___________________________________________________________



















Annexure: 2
Observations and calculations of assay.
Indicator: ___________________
Weight of sample: ____________                                                Factor: ____________
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 purity = volume used by substance x factor x 100
                                                                     Weight of sample

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
g
Grams
ml
Milliliter
oC
Degree centigrade
mg
Milligram
M
Molar
vi
Initial volume
vf
Final volume
Temp.
Temperature
o
Degree (angle)
l
Length
c
Concentration (g/ml)
g/ml
Gram per milliliter
α
Alpha
λ
Lambda


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