25-05-2012, 01:23 PM
SUSPENSION PROTOCOL DISSOLUTION TEST VALIDATION.
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1. LINEARITY
Standard solutions were prepared at 30%-150% of the working concentration for
250mg PARACETAMOL suspension.
Linear regression analysis demonstrated acceptability of the method for quantitative
analysis over the concentration range required
2.ACCURACY
The response of standard solutions at the working concentration for 250mg per mL
is measured and the percent accuracy as determined from the linear regression is
calculated
EXCIPIENT (PLACEBO) INTERFERENCE EVALUATION
The excipients interference was determined by sonicating (15 minutes) a solution of
a paracetamol placebo suspension with an equal paracetamol concentration as the
prepared paracetamol standard solution.
The difference between the response of this artificial solution (containing excipients)
and the standard paracetamol solution as is (without excipients), is stated as
placebo effect.
The placebo effect is calculated from the response of the ration of the excipients
PLUS standard to the standard solution of the same concentration.
Criteria
The placebo effect value should be less than 1.0 - 1.2%
4.METHOD REPEATABILITY
The full method dissolution test as described in the method was carried out on the
finished product
Method repeatability was expressed as relative standard deviation (RSD) of six
independent analyses, each of them performed on six 5mL suspensions samples.
CONCLUSION
VALIDATION CONCLUSIONS
à Repeatability of the dissolution method was proven on batch Lot # 000 (250 mg).
à The results from the Intermediate Precision test do not differ significantly from
those obtained in the method repeatability test .
à Linear regression analysis demonstrated acceptability of the method for
quantitative determinations over the concentration range of 30 % - 150 %.
à The accuracy of the method was demonstrated in the range of 50 % to 100 % of
label amount of the dissolved Active.
à Analysis of the non-active formulation components showed negligible interference
with the quantitative determination of the active substance.
à The standard and stock sample solutions were shown to be stable for at least 24
hours at room temperature and in refrigerator. The stock standard solution was
also shown to be stable for at least 30 days in refrigerator.
à The method was demonstrated to be robust over an acceptably wide working
range of its operational parameters.
The method SI-226-02 for Dissolution testing by UV determination was demonstrated
to be accurate and precise for performing the dissolution testing of said 'Generic'
250mg Tablets.
The method is demonstrated to be suitable for carrying out dissolution test of
Paracetamol suspension .