characterization of raw materials
TRANSCRIPT
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PRESENTED BY
HIBA.C.H
RESHMA FATHIMA.K
FIRST YEAR M.PHARM
DEPT.OF.PHARMACEUTICS
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CHARACTERIZATION OF RAW MATERIALS PHYSICAL CHARACTERIZATION
Bulk properties of API
Solid state properties of API
Intrinsic properties of API
CHEMICAL CHARACTERIZATION
Confirmation of structure of API
Stability Analysis
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Confirmation of
structure of API
Stability/compatibility studies on API/excipient mix ,SolubilityDissolutionChanges on processing
Particlehabit/shape,Particlesize/distributionDensity,Surface area,FlowabilityCompaction
Polymorphism,Solvation,Crystallinity
Solubility,Partitioning/distributionMelting/boiling points/sublimationDissolution
Nuclear magnetic resonance (NMR)Mass spectroscopy,Elementalanalysis
API/excipient mix
Bulk properties of
API
Solid state
properties of API
Fundamental/intrinsic
properties of API
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CONFIRMATION OF STRUCTURE OF API
NMR SPECTROSCOPY
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IR SPECTROSCOPY
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MASS SPECTROSCOPY
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INTRINSIC PROPERTIES OF API
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SOLUBILTY ANALYSIS INCLUDE Pka determination
pH solubility profile
Common ion effects
Effect of temperature
Solubilization
Partition coefficient
dissolution
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Pka determinations Henderson hasselbalch equation
Unionised drug absorbed from the GIT tract
Pka value can be determined by variety of analytical methods.
Spectral shifts by UV or visible spectroscopy
Potentiometric titrations
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Common ion effects common ion effect is defined as the suppression of the degree of
dissociation of a weak electrolyte containing a common ion.
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Effect of temperature
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DISSOLUTION
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Dissolution is the process by which a solute forms
a solution in a solvent. The solute, in the case of solids, has
its crystalline structure disintegrated as separate ions, atoms, and molecules form
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PARTITION COEFFICIENT
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MELTING POINT CAPILLARY MELTING
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HOT STAGE MICROSCOPY
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SOLID STATE PROPERTIES POLYMORPHISM
CRYSTALLINITY
SOLVATION
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DIFFERENTIAL SCANNING CALORIMETRY
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DIFFERENTIAL THERMAL ANALYSIS
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BULK PROPERTIES OF APIPARTICLE SIZE
PARTICLE SHAPE
SURFACE AREA
DENSITY
FLOW PROPERTIES
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STABILITY ANALYSIS
SOLUTION STABILITY
SOLID STATE STABIULITY
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STABILITY IN TOXICOLOGY FORMULATION
Toxicology studies typically commence early in
development, it is often advisable to evaluate samples of
the toxicology preparation for stability and potential
homogeneity problems.
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Solution stabilityThe primary objective of this phase of pre-formulation research is
identification of condition necessary to form a stable solution.
This study include-effect of pH, ionic strength, light, temperature and oxygen
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Solid state stability Solid phase stability depends on several factors like temperature, pH, humidity,
hydrolysis, oxidation, etc
For a new drug compound
Weighed sample are place in open screw cap vials and are exposed directly to light, temp,
humidity for 12weeks.
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INCOMPATIBILITYADAVANTAGE
It helps to avoid surprise problems
TYPES
Physical incompactibility
Chemical incompactibility
Therapeutic incompactibility
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Excipient interaction
Drug –Excipient interactions
Physical interaction
chemical interaction
Biopharmaceutical interaction
Excipient –Excipient interactions
Package –Excipient interaction
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PHYSICAL INTERACTION Tetracycline formed insoluble complex with calcium carbonate leading to
slower dissolution and decreased absorption.
Formulation of chlorpromazine with polysorbate 80 and sodium lauryl
sulphate decreased membrane permeability of drug.
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CHEMICAL INTERACTION Antibiotics, anaesthetics,barbiturates undergo in presence of water low or
high pH.
Steroids, Vitamins, Antibiotics, Epinephrine, Aldehydes, Alcohols, Phenols undergo oxidation reactions
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BIOPHARMACEUTICAL INTERACTIONS Many of the excipients like sorbital, xylitol, have tendency to increase the
gastrointestinal motility thus reducing the time available for absorption of drugs like metoprolol.
Polyethylene glycol 400 also has influence on the absorption of ranitidine
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EXCIPIENT-EXCIPIENT INTERACTIONS Acacia -Ethanol (95%) - Precipitate organic salts of Acacia
Acacia- Ferric and other salts-Mucilage of acacia becomes gelatinous.
Crosscarmellose Sodium- Hygroscopic excipients like Sorbitol Efficacy as disintegrant reduced.
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PACKAGE-EXCEPIENT INTERACTION Glass- Glass containers possess oxides of Boron, Sodium, Potassium,
Calcium, Iron and Magnesium which interact with formulation.
Alter physical and chemical stability of the formulation. E.g.:- sulphate salts react with barium and calcium to form inorganic insoluble
salts.
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Plastic- Moisture uptake
Moisture uptake associated with disintegrants(STARCH) in tablet form microcracks due to disintegrant swelling.
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