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Types of Validation

Submitted to: submitted by:

Dr. GAURAV K JAIN NASR ALI

Pharmaceutics Dep. 1St semester M.pharm.

JAMIA HAMDARD JAMIA HAMDARD

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THE MAJOR TYPES OF VALIDATION :

 Process validation .

 Cleaning validation.

 Equipment validation.

 Validation of analytical methods .
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 Process validation :

 Process validation is the means of ensuring and providing documentary
evidence that processes are capable of repeatedly and reliably
producing a finished product of the required quality.

 pre-requisites for process validation:

 qualification of manufacturing equipment and instruments as well as the

formulation ,this involve compatibility of active ingredients and

recipients and of final product and packaging materials.

 Critical services (water, air, nitrogen, power supply).
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 Equipment cleaning and motivation of personnel.

 

 TYPES OF PROCESS VALIDATION :

(a) PROSPECTIVE VALIDATION.

(b) CONCURRENT VALIDATION.

(c) RETROSPECTIVE VALIDATION.

(d) PROCESS RE-VALIDATION.

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A- Prospective validation:

 is carried out during the development stage by means of a risk

analysis of the production process, which is broken down into

individual steps: these are then evaluated on the basis of past

experience to determine whether they might lead to critical

situations.

 Expected that process validation be completed prior to the

release of the finished product for sale. 5

 

 It includes:-

● Initial stages of formulation development and process development

● Setting of process sampling plans.

● Designing of batch records.

● Defining raw material specifications.

● Transfer of technology from scale up to commercial size batches.

● Environmental controls.

 It is generally considered acceptable that three consecutive
batches within the finally accepted parameters, that assure
product of the desired quality would constitute a proper validation
of the process.

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B- Concurrent validation:

 is used on the batches currently being produced for establishing

documented evidence that a facility and process do what they claim to

do.

 Examples of these may be when:-

 A previous validated process is being transferred to a third party
contract manufacturer or to another site.

 The number of batches produced are limited.

 Process with low production volume per batch and market demand.

 The product is a different strength of a previously validated product
with the same ratio of active or inactive ingredients. 7

 

C- Retrospective validation:

 involves the examination of past experience of production on the

assumption that composition, procedures, and equipment remain

unchanged; such experience and the results of in-process and final

control tests are then evaluated. Recorded difficulties and failures

in production are analyzed to determine the limits of process

parameters.

 Retrospective validation is obviously not a quality assurance measure

in itself, and should never be applied to new processes or products.
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D-PROCESS RE-VALIDATION:

 means repeating the original validation effort or any part of it.

 Process re-validation is required when there is a change in any of the

critical process parameters ,formulation, primary packaging components,

major equipment or premises.

 for examples when:-

 Changes in raw materials:

( physical properties such as density, viscosity, particle size distribution or

changes in source of active raw material manufacturer) 9

 

 Changes in packaging material ( primary container/ closure system).

 Changes in the process (Mixing time, drying temperatures & batch

size).

 Changes in the equipment.

 Changes in the plant/facility.
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 Cleaning validation :

 Cleaning validation ensures that there is no cross contamination in a
multi-product manufacturing plant and also prevents microbial
contamination.

 Objective..

 To minimize cross contamination.

 To determine efficiency of cleaning process.

 To do troubleshooting in case problem identified in the cleaning process

and give suggestions to improve the process.

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 Source of contamination:

 Cross contamination product of one product into another.

 Product contamination by a foreign material.

 Microbial contamination.

 Factors Influencing Cleaning validation :

Product, Equipment, Facilities, Cleaning methods, Cleaning agents,

Sampling, Testing, Limits, and acceptance criteria.

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 Equipment Validation

 Equipment validation is to provide a high level of documented evidence

that the equipment and the process confirm to a standard.

 TYPES:

 DESIGN QUALIFICATION .

 INSTALLATION QUALIFICATION.

 OPERATIONAL QUALIFICATION .

 PERFORMANCE QUALIFICATION.
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 Validation of analytical methods:
 Method validation must prove that the analytical method used for a

specific test is suitable for which it is to be carried out.

 Methods should be validated :-

 When they are to be established for routine use.

 When the method is to be changed due to change in conditions.

 Whenever the equivalence between new method and the standard are

demonstrated 15

 

TYPES OF PROCEDURES TO BE VALIDATED:
1) ACCURACY:-

The accuracy of an analytical method refers to the closeness of agreement
between the observed value and the value which is either conventially a
true one or reference one.

2) PRECISION:-

The precision of an analytical method refers to the closeness of values
obtained from a series of tests.

3) REPEATABILITY:-

Repeatability is established when the same sample is estimated repeatedly
by the same analyst using same analytical method within the same
laboratory using same instrument and performed within a short period of
time. 16

 

4) INTERMEDIATE PRECISION:- When the test is repeated on different days

by different persons or using different instruments within the same

laboratory, the variation is expressed in terms of intermediate precision.

5) REPRODUCIBILITY:- When a method is standardized, the test is carried

out in different laboratories using the same method, the precision

between the laboratories is referred to as reproducibility.

6) SPECIFICITY:- Specificity is the ability of a test method to measure the

analyte explicity in the presence of other components.

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7) LINEARITY:- refers to it’s ability to measure a specific component

within a range.

8) DETECTION LIMIT: the lowest detectable concentration of an analyte

in a sample.

9) QUANTITATION LIMIT:: the lowest measureable concentration of an

analyte in a sample.

10) ROBUSTNESS: ability of a test method to resist the variation in

method parameters ( small variation).

11) RANGE: interval between upper and lower concen. Of analyte.
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