validation of analytical procedures

7/29/2019 Validation of Analytical Procedures

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Validation Of Analytical

Procedures

ILDA MONALISA

INDUSTRY OF PHARMACY


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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).


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Objective

The objective of validation of an analitycal procedure

is to demonstrate that it is suitable for its intended

purpose.


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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.


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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


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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.


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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.


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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)


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Characteristic of Validation

Accuracy

Precision

Robustness

Specificity Detection limit

Quantitation limit

Linearity

Range


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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.


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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.


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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.


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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.


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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.


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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.

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