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VALIDATION OF RAW MATERIAL

Mardiyati Hasanah
1111013018
Kelas B
DEFINITION OF RAW MATERIAL
RAW MATERIAL: It is a term used to denote
starting materials, reagents and solvents
intended for use in the production of
intermediates or active pharmaceutical
ingredient(API).
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Validation of raw material
Validation begins with the raw materials,
active pharmaceutical ingredients excipients
Raw materials, major causes of product
variation or deviation from specification
Most uncontrollable component in the
complete product/process validation scheme
because morphology particle size/surface area
not be completely defined this early

It includes validation of both active
ingredients & excipients
Characteristics - particle size, surface area,
color, density.
Chemical characteristics- water content
residue on ignition & heavy metals
Variables: Flow, blend uniformity, granulation
solution/binder uptake compressibility,
lubricant efficiency.
RAW MATERIALS & ITS IMPORTANCE
Chemical characteristics : Drug impurities can
affect the stability.
Physical properties: Drug morphology, solubility
& particle size/surface area may affects drug
availability.
The particle size, shape , and density can affect
material flow and blend uniformity.
The hygroscopic drug caring in handling the
material and the reproducibility of the
manufacturing process.
STEPS FOR RAW MATERIALS
VALIDATION
1. Each raw material validated by testing at least 3
batches from primary & alternate supplier ;
representing the ranges, both high and low.
2. Depending on the susceptibility aging, physical,
chemical, and/or microbiological stability should be
assessed.
3. If under acceptable range, especially for materials
sensitive to small changes; then appropriate to use
several lots of raw material with low and high ends of
the specification.
4. The final step of raw material validation should
involve an on-site inspection of the vendors to review
the manufacturing operations, controlling &
conforming to
RAW MATERIAL VALIDATION
Several steps are required to validate a raw material. They are as
follows:

(1) LIST ALL THE RAW MATERIALS NEEDED TO
PREPARE A PRODUCT BATCH.

The list should include the materials used in production and testing
Active ingredients
Excipients
Processing aids
Chemicals
Official standards
Laboratory materials

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(2) IDENTIFY AT LEAST TWO SUPPLIERS FOR EACH
RAW MATERIAL.
After we have complete list of all raw materials needed, we
must locate sources of these materials.
It is always advisable to locate and validate at least two
suppliers.
EVALUATION FOR SELECTING A SUPPLIER:
(1)Provide the raw material that we need
(2)Must be capable of providing the grade that we want
(3)Providing the quantity that we require
(4)To provide increased quantities quickly (to evaluate the
supplier s capacity)
(5)Determine whether our supplier is a manufacturer or
distributor?

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(6) Cost of the raw material.
(7) Reputation and reliability of the supplier.

NOTE: He must use written standard operating procedures and
establish proper raw material storage conditions and distribution
procedures.
Precautions
Joint agreements
Attention
Investigation
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(3) IF A SUPPLIER IS NEW, VISIT HIS FACILITY.

It is important to establish a good relationship with a
supplier.

To meet representatives personally.

Inspect his facility.


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During the visit, it is also important to observe..
housekeeping and sanitation practiced
The use of written procedures and logs
proper segregation and batch identification
The use of laboratory notebooks
The size of the laboratory area and staff
The use of up to date laboratory instrumentation and
production equipment.


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(4) OBTAIN SAMPLES AND SUPPLIERS CERTIFICATES
OF ANALYSIS

To determine the characteristics of the raw material.

The certificates of analysis and samples the extent of
variation from lot to lot on specific tests.

It is important to measure this variation between different lots
from the same supplier and then the variation between suppliers.
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(5) ESTABLISH SPECIFICATIONS FOR EACH RAW
MATERIAL
List of parameters.

For each parameter listed, an acceptable , measurable range of
activity should be established.

Compendial raw materials

And non- compendial raw materials

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(6) ESTABLISH TEST PROCEDURES.
A test procedure must be established for each specification.
For raw materials that are compendial, test procedures are
denoted along with their respective specifications.
For raw materials that are not listed in official compendia,we
embark into methods development.
This work calls on compendial methods that exist for similar
compounds, which can be modified. It also calls for methods that
are published literature.
Documentation of so developed test procedures should be paid
attention.
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(7) ESTABLISH SAMPLING PROCEDURES.
Documentation of raw material sampling is developed.
This procedure includes general requirements that may apply to
any raw material received in the plant, such as
The number of containers to sample(sample size).
Method of sampling.
Individual raw materials may have certain sampling
requirements based on their stability and/or intended use.
Before these individual sampling procedures are instituted in
routine practice, they should be evaluated as part of process
validation.
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(8) ESTABLISH OPTIMUM STORAGE CONDITIONS
Raw material containers must be handled and stored under
prescribed conditions in order to protect their stability over the
stated shelf life.
The chemistry of each raw material should be reviewed and
aspects concerning hygroscopity, sensitivity to light,sensitivity to
high and low temperature extremes, ability to support microbial
growth,reactivity with any container or closure system, and
oxidising capability are checked.
Once we have established the factors that critically affect a raw
material, we can conduct stability studies that will indicate the
optimum storage conditions and establish a shelf life for the raw
material.
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(9) ESTABLISH SHELF LIFE
Shelf life or expiry dating of a raw material is the time period
within which it must be used.

Some times we assign an expiry date that is shorter than our
data indicate, so that we will always use fresh raw materials.

The shelf life of a raw material is established by testing over
time in the containers and closures to be used, after storage under
the anticipated optimum conditions, and also under adverse
conditions.

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(10) CHALLENGE OF THE RAW MATERIALS.

The last step required to validate a raw material is the
operation in which the information that has been established
concerning the raw material is challenged, to assure that is
scientifically sound and meaningful.

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To build up quality in the final product a thorough control over
each step of the process is required.
This makes it essential to establish a documented evidence to
be developed by thorough experimentation.
So the raw materials are not an exception to this and they
should be validated by opting an systematic approach.



CONCLUSION
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REFERENCES
Robert A. Nash, pharmaceutical process validation.
Berry, I.R.,and Daniel harpaz, validation of active pharmaceutical
ingredients.
P.P.sharma, how to practice GMPS.
Validation in API manufacturing plants.Brussels:active
pharmaceutical ingredients committee. http://www.apic.ecfic.org
Guide to Inspections Validation of Processes. Washington DC:use
Food and Drug Administration.
http:/www.fda.gov/ora/inspect_ref/igs/valid.html.
Validation of compendia Methods.The United States Pharmacopeia
Convention,Inc.,1995.
A Seminar on Validation of Solid Dosage Forms by Naincy Gupta
M.Pharm (IInd Sem) Pharmaceutics.


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