DACLATASVIR SOP


DACLATASVIR SOP

1.0  OBJECTIVE:
To lay down a procedure for the active raw material of the Daclatasvir 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  Assay:
5.1.1        Apparatus:
5.1.1.1  Glassware (according to requirement).
5.1.1.2  Potentiometer.
5.1.2        Material and reagents:
5.1.2.1  10.0ml of anhydrous acetic acid.
5.1.2.2  0.1M Perchloric acid.
5.1.2.3  Crystal violet solution (as indicator).
5.1.3        Sample:
5.1.3.1  0.12g of Daclatasvir.
5.1.4        Method of analysis:
5.1.4.1  Take a 100.0ml of beaker and add 0.12g of sample in it.
5.1.4.2  Add 60.0ml of anhydrous acetic acid R in it and dissolve by using magnetic stirrer i.e. SOP
5.1.4.3  Fill the right hand side burette with titrant 0.1M Perchloric acid.
5.1.4.4  Carry out a Potentiometric titration using crystal violet solution as an indicator.
5.1.4.5  Operate potentiometer according to SOP.
5.1.4.6  To neutralize analyte add titrant fixed volume (1ml, 0.5ml or 0.1ml) from burette every time note the reading of change in potential difference (millivolts) for each addition in given annexure-1.
5.1.4.7  Plot a graph, volume used v/s millivolts.
5.1.4.8  Find out the END POINT.
5.1.4.9  Peak of graph indicates END POINT i.e. the point at which maximum millivolts. Note down volume used at that point.
5.1.4.10    Perform blank titration without using sample. Similarly, as sample titration performed. Record observations in annexure-1.
5.1.4.11    Calculate volume used by substance by using formula:
Volume used by substance = Blank titration - Sample titration.
5.1.4.12    Calculate percentage purity of the sample by using formula:
%age purity = volume used by substance x factor x 100
                                                  Weight of sample
5.1.5        Factor:
5.1.5.1  1ml of 0.1M Perchloric acid is equivalent to 74.64mg of Daclatasvir.
5.1.6        Limit:
5.1.6.1  98.0% to 102.0% (anhydrous substance).
6.0  REVISION LOG:
Revision No.
Effective Date
Reason
00

New SOP

7.0  REFERENCES:
7.1  Manufacturer’s specifications.
8.0  ANNEXURES:
Annexure 1: Assay observations and calculations (Potentiometric titration).


Annexure: 1
Assay observations and calculations (Potentiometric titration)
Potentiometric titration
Reference electrode: ___________________
Indicator electrode: ____________________
Speed of magnetic stirrer: _______________
Titrant used: __________________________
Indicator: ____________________________
Blank titration:
Sr.#
Volume used
(ml)
Voltmeter
(mV)












Plot a graph, volume used v/s millivolts and find out peak of graph i.e. END POINT of blank titration.
Sample titration:
Sr.#
Volume used
(ml)
Voltmeter
(mV)












Plot a graph, volume used v/s millivolts and find out peak of graph i.e. END POINT of sample titration:
Volume used by Blank titration: __________________
Volume used by Sample titration: _________________
Volume used by substance = Blank titration – Sample titration.






mV used by Blank titration: __________________
mV used by Sample titration: _________________
mV used by substance = Blank titration – Sample titration.




Volume used by substance: _______________________
Voltmeter (mV) used by substance: _________________










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
QCEO
Quality control Equipment (Operation).
v/s
Verses
mV
Millivolts
g
Grams
ml
Milliliter
mg
Milligram
M
Molar
%
Percentage
R
Reagent


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