Validation profile sahil

SHRI BMCPER, MODASA NIKITA 11

Seminar on

VALIDATION PROTOCOLS

DEPARTMENT OF PHARMACEUTICSSHRI B. M. SHAH COLLEGE OF PHARMACEUTICAL EDUCATION AND

REASERCH, MODASA-2013

GUIDED BY: Dr. M. R. PATELPrincipale & HOD in pharmaceutics

PRESENTEDE BY:

SAHILHUSEN I . JETHARAM. PHARM – I (2013-14)ROLL NO. - 02

SHRI BMCPER, MODASA NIKITA2

LIST OF CONTENTS………

INTRODUCTION TABLETSPHARMACEUTICAL POWDERSORAL LIQUID SEMISOLID DOSAGE FORM

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INTRODUCTIONVALIDATION

It is a documented programme which provides a high degree of assurance that a specific process will consistently produce a product meeting its predetermined specifications & quality attributes.

Why validation is required? Manufacturers require by law to conform to cGMP. To avoid possibility of rejected or recalled batches.

- To ensure the product uniformity , reproducibility, &

quality

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Validation Protocol

It gives Details of the critical parts of the of the

manufacturing process. Information about the key parameters that are

to be measured. Allowable range of variability in case of

measured parameters. The manner in which the system will be tested.

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Types of validation Prospective Validation:- an experimental protocol is

run before starting of actual use. Concurrent Validation:-In process monitoring of critical

processing steps & end product testing of current production

Retrospective Validation:-It is chosen for established products where their manufacturing processes are considered to be stable ( i.e. long history state of control)

Validation is done for.:- a) Raw materials

b) Process

c) Product.

TABLETS


It is unit solid dosage forms containing drug substances with or without suitable diluents and prepared by compressing powdered or granulated medicinal substances in die.

Validation

IN CASE OF TABLETS IT IS DONE FOR:-

1. RAW MATERIAL

2. PROCESS

3. PRODUCT

4. FINISHED PRODUCT


RAW MATERIAL VALIDATION:- Raw material is validated for particle size, surface area,

particle size distribution, colour , Appearance, texture, density, flowability , compressibility etc

PROCESS VALIDATION:-

Two stage First identify the critical process parameter and design

protocol Manufacture three batches of product controlling the

critical parameter and test it for complianceSHRI BMCPER, MODASA NIKITA

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PRODUCT VALIDATION:-


1. Raw Material2. Packaging Material3. Granules 4. Compressed Tablets5. Coated Tablets6. Packed Final Product

FINISHED PRODUCT VALIDATION:-1. ORGANOLEPTIC PROPERTY2. PHYSICAL CHARACTERISTIC3. CHEMICAL CHARACTERISTIC4. BIOLOGICAL CHARACTERISTIC5. MICROBIOLOGICAL CHARACTERISTIC6. STABILITY TESTING7. STORAGE CONDITION

SHRI BMCPER, MODASA NIKITA

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PHARMACEUTICAL POWDERS

API + EXCIPIENT POWDER (BOTH ARE IN POWDERED FORM) DOSAGE FORM

Powder are homogeneous mixture of drug/drugs and excipient/excipients in a dry, fine state of subdivision.

It is important to note that term" POWDER” is restricted only to “POWDERS FOR INTERNAL USE ONLY”.

But not used for other powder mixtures. For EX. like powder for external use they rather called as “Dusting powders”.

SHRI BMCPER, MODASA NIKITA

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POWDERS AS A PRIMARY REQUIREMENT FOR DOSAGE FORM

VALIDATION1. Validation of Raw material

2. Validation of Blending Equipments

3. Validation of Blending operation

4. Validation of final packed material


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1. VALIDATION OF RAW MATERIAL

Physical characteristics of raw material can vary among manufacturers of drug substances.

Inspection should cover the firm’s data for the specification for drug substances.

RAW MATERIAL SPECIFICATION Description, identification, melting range, ph, water,

residue on ignition, chloride, sulfate, sulfide, heavy metals, readily carbonizable substances, total aerobic microbial count, mould and yeast count, E. Coli, acceptable container, approved expiry date, approved suppliers.

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2. VALIDATION OF BLENDING EQUIPMENTS

What is the working capacity of equipment? Does the equipment operate more efficiently with the density

of fluffy powders? What is the working load range, i.e. the proper blender load to

ensure good uniformity of blend? What feature does the equipment have for ease of handling of

powders, automated charging and discharging Can the equipment heat the powder blend if needed for

application as a dryer as well as a granulator? Is the method of heating electric or steam?

May a vacuum be used with the equipment? Does the equipment have the capacity to wet the powder

blend?

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3. Validation of Blending

operation

Determination of the optimum blending time De-mixing or segregation Verification of homogeneity of mixed powders Interaction between process & material Validation of characteristics of blend. -Bulk density -Particle size distribution -Moisture content Load size in blending apparatus Powder flow

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4. Validation of final packed material

Checking integrity of foils

Checking integrity of sealing

Checking opening ease

Permeability of foils

Classification

1. PROCESS VARIABLES

2. PRODUCT VALIDATION


1. Process VariablesProcess Equipme-

ntsProcess variables Properties

affected by variables

Monitoring output

Mixing of

liquid

Kettle & Tank fitted with agitator

Capacity of unit,

Shape & position

of agitation system,

Order of addition,

Rate of addition,

Fill volume,

Mixing speed of agitator,

Temperature of liquid,

Mixing time.

Appearance of liquid, Viscosity of liquid.

Potency, Appearance, pH,

Viscosity, Specific gravity.

Process Equipment Process variables

Properties affected by variables

Monitoring output

Dispersing Homogenizer, Colloid mill, ultrasonic device

Bore opening/

clearance of rotor & stator/power setting,

Pressure/rotor speed/power consumption,

Feed rate,

Temperature,

Dispersion time,

Order of mixing.

Particle size of solids,

Viscosity of liquid.

Potency,

Particle size

Distribution,

Viscosity,

Specific gravity.

2. PRODUCT VALIDATION

Major test parameters used for final product testingAppearance

pH

Viscosity

Specific gravity

Microbial count

Leakage test for filled bottle (By plastic vacuum dessicator)

Check the cap sealing

Fill volume determination

Particulate matter testing

Water vapour permeability test

Stress test

Test parameters specific for suspension • Sedimentation rate• Resuspendibility• Particle size & particle size distribution• Zeta potential measurement

Type of emulsion determination by• Dilution test • Conductivity test• Dye solubility test• COCl2 filter paper• Fluorescence test• Direction of creaming

Test parameters specific for solution • Clarity of solution• Color of solution


Semisolid Dosage Form

Process validation protocol

Contents

1. Protocol Approval2. Objective3. Scope4. Validation Approach5. Document Required 6. List of Equipments7. Product Detailed8. Parameter to be tested9. Sampling plan10. Acceptance Criteria

NameName DesignationDesignation SignatureSignature

Prepared ByPrepared By

Checked ByChecked By

Approved ByApproved By

ABC Pharmaceuticals.27, Mahalaxmi Estate, Vatva, Ahmedabad.

Prepared by Checked by


5. Document required DocumentDocument Effective Date Effective Date Ref. No.Ref. No.

MFRMFR

BMRBMR

BPRBPR

Test data sheetTest data sheet

6. List of equipments

7. Product detailed

Generic name: Brand name: Product description: Dosage form: Labeled claim: Category: Composition with specification:



8. Parameters to be tested



Process stageProcess stage Process variableProcess variable Validation responseValidation response

1)1) MixingMixing a)a) Mixing timeMixing time

b)b) Mixing rateMixing rate

c)c) Mixing temp.Mixing temp.

→→By assayBy assay

→→Consistency TestConsistency Test

2)2) FillingFilling a)a) Filling rateFilling rate

b)b) SpeedSpeed

→→Weight variationWeight variation

→→Sealing temp.Sealing temp.

→→Pressure, CrimpingPressure, Crimping

→→Coding.Coding.

9. Sampling plan



Process StageProcess Stage No. of sample No. of sample takentaken

Qty Qty TestTest

1) Mixing1) Mixing 22 30 gm from 30 gm from each locationeach location

Qty of sample Qty of sample takentaken

TestTest

2) Filling2) Filling Equivalent to no Equivalent to no of filling stationof filling station

10. Acceptance criteria



StageStage TestsTests Acceptance CriteriaAcceptance Criteria

1) Mixing1) Mixing Assay of ingredientsAssay of ingredients

Consistency testConsistency test Spread smoothly & Spread smoothly & homogeneouslyhomogeneously

2) Filling2) Filling FOR FOR 15 gm15 gm

Wt of empty tubeWt of empty tube

Wt of filled tubeWt of filled tube

Net contentNet content

Crimping Crimping

CodingCoding

Sealing Sealing

Sealing temp.Sealing temp.

Air trappingAir trapping

Pressure Pressure

Assay of ingredientsAssay of ingredients

LegibleLegible

Straight & SmoothStraight & Smooth

Complete & Leak proofComplete & Leak proof

280280°°C – 300C – 300°°CC

Free from air bubbleFree from air bubble

3.5 – 4.0 Kg/cm3.5 – 4.0 Kg/cm22


REFERENCES

Pharmaceutical process validation by Loftus and.Nash


Ph. No. :- +918460378336Address:- 44, Assiyana Society; Dugarvada Road, Taluko & City : Modasa State: Gujarat Country: IndiaEmail: [email protected]

BEST OF LUCK TO ALL . . . . . . . . . .

Validation profile sahil

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