7/29/2019 Validation of Analytical Procedures
1/15
Validation Of Analytical
Procedures
ILDA MONALISA
INDUSTRY OF PHARMACY
7/29/2019 Validation of Analytical Procedures
2/15
Definition
Validation Of Analytical Procedures is anassessment of the actions of certain parameters
based on laboratory experiments to prove that
these parameters satisfy the requirements for use
(Harmita,2004).
7/29/2019 Validation of Analytical Procedures
3/15
Objective
The objective of validation of an analitycal procedure
is to demonstrate that it is suitable for its intended
purpose.
7/29/2019 Validation of Analytical Procedures
4/15
Types of Analytical Procedures to be
Validated
The discussion of the validation of analyticalprocedures is directed to the four most common
types of analytical procedures:
A. Identification test
B. Quantitative test for impurities contentC. Limit tests for the control of impurities, and
D. Quantitative test of tg active moeity in samples of
active pharmaceutical ingredient (API),
pharmaceutical product or other selected
component in the pharmaceutical product.
7/29/2019 Validation of Analytical Procedures
5/15
A. Identification Test
Indetification tests are intended to ensure theidentify of an analyte in a sample. This is normally
achieved by comparison of a property of the
sample (e.g, spectrum, chromatographic
behaviour, chemical reactivity, etc) to that areference standard
7/29/2019 Validation of Analytical Procedures
6/15
B. Testing for impurities
Testing for impurities can be either a quantitativetest or a limit test for the impurity in a sample.
Either test is intendedto accurately reflect the
purity characteristic of the sample. Different
validation characteristics are required for aquantitative test than for a limit test.
7/29/2019 Validation of Analytical Procedures
7/15
C. Quantitative Test of the Active
moiety in samples of API
Assay procedures are intended to measure the
analyte present in a given samples. In the context of
this document, the assay represents a quantitative
measurement of the major component in the API.
7/29/2019 Validation of Analytical Procedures
8/15
For the pharmaceutical product, similar validation
characteristics also apply when assaying for the
active or other selected component. The same
validation characteristic may also apply to assays
associated with other analytical procedures (e.g.Dissolution)
7/29/2019 Validation of Analytical Procedures
9/15
Characteristic of Validation
Accuracy
Precision
Robustness
Specificity Detection limit
Quantitation limit
Linearity
Range
7/29/2019 Validation of Analytical Procedures
10/15
A. Accuracy
Accuracy is a measure of the degree of closeness
of the results of the analysis with the actual levels
of analyte. Accuracy is expressed as the percent
recovery added analyte.
B. Precision
Precision is a measure that indicates the degree of
fit between the individual test results as measured
by the spread of individual results from the averageif the procedure is applied repeatedly in samples
taken from a homogeneous mixture.
7/29/2019 Validation of Analytical Procedures
11/15
C. Robustness
To validate the robustness of the method needs tobe made smaller and metodologiyang changes
continuously and analytically evaluating the
response and the effects of precision and accuracy.
D. Specificity
Specificity is its ability to measure only certain
substances careful and thorough in the presence of
other components that may be present in the samplematrix.
7/29/2019 Validation of Analytical Procedures
12/15
E. Limit Of Detection (LOD)LOD is the smallest amount of analyte in a sample
that can be detected are still significant response
compared to the blank.
F. Limit Of Quantitation(LOQ)
LOQ is a parameter in the analysis of trace and
defined as the smallest quantity of analyte in a
sample that can still meet the criteria of careful and
thorough.
7/29/2019 Validation of Analytical Procedures
13/15
G. Linearity
Linearity is the ability of the analytical methods thatrespond directly or with the aid of a good
mathematical transformation, proportional to the
concentration of analyte in the sample.
H. Range
Range is the lowest and the highest expression of
analytes that have been shown to be set with
accuracy, precision, and linearity is acceptable.
7/29/2019 Validation of Analytical Procedures
14/15
Revalidation
Furthemore revalidation may be necessary in thefollowing circumstances:
Changes in the synthesis of drug substance
Changes in the composition of the finished
product, and
Changes in the analtycal procedure.
7/29/2019 Validation of Analytical Procedures
15/15
Reference
Anonim,2006. Pedoman Cara Pembuatan Obatyang Baik. Jakarta: Badan POM, 122-124.
Harmita, 2004. Petunjuk Pelaksanaan Validasi
Metode dan Cara Perhitungannya. Majalah Ilmu
Kefarmasian, Vol.1, No.3, Desember 2004.
Top Related