validation parameters for solid dosage form

1. GOVT COLLEGE OF PHARMACY
AMRAVATI
TOPIC:-
“VALIDATION OF SOLID DOSAGE FORMS”
Prepared By:-
A.R KHAN
M.PHARM 1ST YEAR
(Q.A)
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2. Introduction:-
• Validation is a systematic approach to identifying,
measuring, evaluating, documenting, and re-
evaluating a series of steps in the manufacturing
process to ensure a reproducible final product.
• According to US-FDA, 1987
“Process Validation” is establishing documented
evidence which provides a high degree of
assurance that a specified process will consistently
produce a product meeting its pre-determined
specifications and quality characteristics.”
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3. 3
Types of process
validation
PROCESS
VALIDATION
RETROSPECTIVE
PROCESS
VALIDATION
PROSPECTIVE
PROCESS
VALIDATION
CONCRURREN
T PROCESS
VALIDATION

4. PRODUCT VALIDATION
product validation involves following steps:
• validation of raw materials and excipients.
• analytical methods of validation.
• equipment and facility validation .
• process variables and limits.
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5. VALIDATION OF RAW
MATERIALS AND EXCIPIENTS
The validation process of solid dosage form begins
with the validation of raw materials ,both API and
excipients.
• validation of raw materials is one of the major causes
of product variation or deviation from specification.
• preformulation is one of the critical step to be
validated in product validation
-Physical characters such as drug and particle size
can affect material flow and blend uniformity.
-Chemical characters like impurities can effect
stability of drug.
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6. 6
Excipients can represent less then 1% of a tablet
formula
Factors to be aware of are
• The grade and source of the excipients
• Particle size and shape characteristics and
• Lot-to-lot variability
VALIDATION OF EXCIPIENTS-

7. VALIDATION OF
ANALYTICAL METHODS
• Accuracy of method:
• Precision of method:
• Specificity:
• Repeatability
• Reproducibility:
• precision:
• Ruggedness:
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8. EQUIPMENT VALIDATION -
This protocol can be divided into
• Design qualification
• Installation qualification
• Operation qualification
• Performance qualification
• Maintaince (calibration, cleaning, repair) qualification
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9. 9

10. Validation of tablets
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11. Validation protocol for tablets
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12. INDUSTRIAL PROCESS FOR
SOLID DOSAGE FORMS
Steps &Process parameter are following-
1.MIXING OR BLENDING
Techniques- 1.Diffussion(tumble)
2.convection(planetary or fluid bed).
Mixing and blending depends upon various factors-
1.Mixing speed
2.Mixing Time
3.drug and excipient uniformity
4.equipment capacity
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13. EQUIPMENTS-
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14. 2.WET GRANULATION
what type of wet granulation to be used
LOW SHEAR
HIGH SHEAR
wet granulation parameters are
• Binder addition-
• Binder conc-
• Amount of binder solution-
• Granulation end point-
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15. EQUIPMENTS-
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16. 3.WET MILLING
Does the wet granulation needs to break up the lumps
and enhance the drying of granulation
factors –
• screen size
• mill speed
• feed rate
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17. EQUIPMENTS-
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18. 4.DRYING
Drying is a most important and It is important to keep
the residual moisture low to prevent product
deterioration and ensure free flowing properties.
factors-
• Inlet/outlet temp-
• Airflow-
• Moisture uniformity-
• Equipment capacity-
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19. EQUIPMENTS-
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20. 5.LUBRICATION
Factors:-
1.selection of lubricant-
2.amount of lubricant-
3.mixing time-
The compression is done either by single punch machine
(stamping press) or by multi station machine (rotary press).
factors-
• compression speed-
• compression or ejection force-
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6.TABLET COMPRESSION

21. EQUIPMENTS-
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22. In process test in compression
The following in-process tests should be examined during the
compression stage-
• Appearance
• Hardness
• Tablet weight
• Friability-0.5-1%
• Disintegration
• Weight uniformity
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23. 7.THE TABLET COATING
PROCESS
Many solid pharmaceutical dosage mediums are
produced with coatings, .
key areas –
• equipment type- (convectional or perforated
pan and fluid bed coaters are potential.)
• pan speed-.
• spray rate-
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24. EQUIPMENTS-
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25. APPEARANCE TEST FOR TABLET COATING
• cracking or peeling of the tablet
• intagliation fill-in
• color uniformity
• coating efficiency should be determined for the
coating operation
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26. • Moisture content of dried
granulation- usually less
then 2%
• Granulation particle size
distribution
• Individual tablet weight
• Tablet hardness
• Tablet thickness
• Disintegration
• Impurity profile
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8.TESTS
IN PROCESS TESTS FINISHED PRODUCT TESTS
• Appearance
• Assay
• content uniformity
• Tablet hardness
• Tablet thickness
• Impurity profile
• dissolution

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Validation of capsules

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29. CAPSULE COMPOSITION
• 1.capsule shell provide – the presence of each ingredient in the
capsule formulae. Justify the level and grade of each
ingredient .
• Explain the selection of the capsule size and shape
• Discuss the need for capsule identification(color).
• 2. capsule shell contents- establish the compatibility of the
capsule shell and the capsule contents.
• Determine the hygroscopic nature of the capsule formulation .
• For example, a hygroscopic formulation(API /excipients)can
pull water from the capsule shell, which could effect the API
stability.
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30. 30
EQUIPMENTS

31. PROCESS EVALUATION AND
SELECTION
• The process to manufacture the contents of a hard
gelatin capsule is the same as the tablet. It may
required only a blending step, such as a direct
compression tablet, or such as a wet granulation tablet
(eg mixing, wet milling, drying, dry milling and
blending).In either case, the materials are then
encapsulated in a capsule shell.
• ENCAPSULATION-
• Encapsulation is a critical step in the production of
capsules, similar to the compression for tablet dosage
forms. The materials to be encapsulated will need to
have good flow properties and a consistent density. 31

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Quality control tests
PHYSICAL TEST
• Disintegration test
• Weight variation
CHEMICAL TEST
• Dissolution test
• Assay
• Content uniformity
• Stability testing
• Moisture permeation
test
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33. • Solid dosage form validation should be part of comprehensive
validation program within an industry.
• The validation team must identify the product and process
characteristics to ensure that product will meet all quality,
manufacturing and regulatory requirements.
• Continuous awareness of validation will produce
reproducibility.
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CONCLUSION

34. REFERENCE
• http//www.pharmainfo.net/reviews/guidelines-general-
principles-validation-solid-dosage.
• Berry I.R., and Nash R.A., ”Pharmaceutical
Process validation” second edition, revised and
expanded; Marcel Dekker series; 83-110
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35. Start Each Day LIKE its
your BIRTHDAY…….
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