Transcript Guidelines
Pharmaceutical Development with Focus
on Paediatric formulations
WHO/FIP TRAINING WORKSHOP
Hyatt Regency Hotel
Sahar Airport Road, Andheri East,
Mumbai, India
28 April 2008 – 2 May 2008
1|
Snehal Khedkar | April 2008
Greetings from
Ipca
Ipca Laboratories Limited
Partnering Healthcare Globally
2|
Snehal Khedkar | April 2008
Pharmaceutical Development with Focus
on Paediatric formulations
Practical problems in developing FDCs
& Bilayer tablets
Presenter: Snehal Khedkar
Email: [email protected]
3|
Snehal Khedkar | April 2008
Practical problems in developing FDCs & Bilayer tablets
What are Fixed Dose Combinations???
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Snehal Khedkar | April 2008
Practical problems in developing FDCs & Bilayer tablets
Fixed Dose combination (FDC)
“ A combination of two or more actives in a fixed ratio
of doses.”
Source: WHO Technical report series, No. 929, p.no-107, 2005
Examples of FDCs in WHO’s list of essential drugs
Anti- Infective:
Sulfamethoxazole + Trimethoprim
Anti-Tuberculosis: Rifampicin + Isoniazid
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Antiviral:
Stavidine + Lamivudine + Neviparine
Antimalarial :
Artesunate + Amodiaquine
Snehal Khedkar | April 2008
Rationale….
Reduced Pill Burden
Patient Convenience
Patient Adherence
Monotherapy prevented
Least probability of developing
drug resistance
Validated theory with other
infectious diseases like TB,
Leprosy, AIDS.
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Snehal Khedkar | April 2008
Rationale….
Co-morbid
Conditions
Hypertension
Heart Disease
Diabetes
Obesity
Hyperlipidemia
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Snehal Khedkar | April 2008
Treat different ailments in the
same patient (co-morbidity), at
the same time and with one pill
Allows for synergistic
combination
Rationale….
POLY -PHARMACY
Diabetes
Tuberculosis
Hypertension
Malaria
Allergy/Asthma
AIDS
Ulcers
Pain
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Snehal Khedkar | April 2008
Combination drugs that target
the same indication
Rationale….
SIDE EFFECTS
Weight
Gain
Reduced by using one drug of the
combination for this purpose
Stomach
Irritation
Nausea
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Snehal Khedkar | April 2008
Amiloride may prevent hypokalemia
caused by hydrochlorthiazide
Challenges in Development of FDCs
“Manufacturing challenges:
Product Formulation issues
Manufacturing issues
10 |
Snehal Khedkar | April 2008
Product Formulation issues ……
Problems…
Solutions…
Disproportionate doses
e.g. Metformin + Glibenclamide
(400 mg + 2.5 mg)
- Content uniformity
Dilution for low dose drug
Drug loading / Adsorption on
excipients
- Assay
Different release kinetics
e.g. Rabeprazole + Domperidone
(20 + 30 mg)
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Snehal Khedkar | April 2008
IR +SR (Use of OCRS)
Bilayer/ Trilayer
Product Formulation issues ……
Problems…
Solutions…
Hygroscopicity
e.g. Metformin + Glipizide
Metformin- Poorly compressible
Needs residual moisture
Glipizide - Degrades in moisture
Separate granulation
Coat the Glipizide particles
Altered solubility/ stability
e.g. Atorvastatin + Ramipril + Aspirin
Synergistic action
Atorvastatin -is acid labile
Aspirin- Undergoes alkaline hydrolysis
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Snehal Khedkar | April 2008
Suitable excipients
Drug Delivery Systems for FDCs…..
Matrix system
Multilayered tablets
(bi/tri)
Compression coated
Tab-in-tab
In-lay technology
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Snehal Khedkar | April 2008
Delivery systems to formulate FDCs…..
Multiple unit system
Beads / coating
Particulate / Coating (MUPS)
Multicompartment capsules
Capsule within capsule
Capsule – coated
Mini-tab in capsules
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Snehal Khedkar | April 2008
Dual Release Drug Absorption Systems
Multi-layered tablets
Bilayer, Trilayer & Tab -in -Tab
One or more than one drug combination with
different release patterns
Incompatibility, stability issue can be resolved
15 |
Snehal Khedkar | April 2008
Multilayered Tablets…..
Bilayer Tabletting
+
Release of both drugs starts immediately
Ease of manufacturing
Elegance to the product
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Snehal Khedkar | April 2008
Multilayered Tablets…..
Trilayer tabletting
Inert layer
+
+
Two incompatible drugs
Combination of incompatible drugs
Combination of different release profiles
Elegance to the product
17 |
Snehal Khedkar | April 2008
Problems in layered tablets…..
Lack of proper bonding of two layers
100,000 tablets
several days
200,000 layers
Stress due to high compression force
degrades certain actives e.g. ramipril
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Snehal Khedkar | April 2008
Probable cause of
increase in impurities
Crystal lattice ruptures
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Snehal Khedkar | April 2008
Tablet-in- Tablet Technology…..
Tab-in-Tab
Elegance to the product
Improved product stability
Minimal incompatibility
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Snehal Khedkar | April 2008
Inlay Technology…..
A new platform technology for decreasing the mechanical
shear on double compressed products which can lead to
decrease in unknown/process related impurities.
Release of both drugs starts immediately
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Snehal Khedkar | April 2008
Case study……Artemisinin based FDCs
Artesunate + Amodiaquine HCl
Dosing regimen based on weight to age data
Optimised dose ratio i.e. 1 : 3
Rationale: To ensure that patients take both drugs together in the right dose,
with a particular attention paid to paediatric needs (dose ratio, age-adapted
strengths, optimized pharmaceutical formulation)
Ref: WHO Bulletin, Vol 84, No. 12 Dec. 2006, 921-1000
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Snehal Khedkar | April 2008
Chemical incompatibility…..
ACID –DEGRADED ARTESUNATE
AMODIAQUINE. HCl
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Snehal Khedkar | April 2008
ARTESUNATE
Technology Used ……
A’sunate
(Optionally coated)
A’quine
Bilayer technology
Limited contact
Degradation problem solved
24 |
Snehal Khedkar | April 2008
Critical Process Parameters ……
Sr.
No.
Parameters
1
API
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Remark
i. Particle size
distribution
Increase in effective surface area
ii. Storage
Protect Artesunate from moisture
2
Granulation Point
Wet mass (mixing time)= Improved wetability
3
Moisture Content
Less than 1%w/w
(Measured on IR
moisture balance at
65ºC)
Improvement in compaction properties
4
Hardness of Tablets
Low
High
Snehal Khedkar | April 2008
Layer separation
Decrease in Solubility/ Dissolution
Evaluation studies ……
Stability Indicating Assay
Related Compounds
Dissolution Profile
Content Uniformity
OVI / Residual Solvents
Impurity profile study
Drug : Excipients
compatibility study
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Snehal Khedkar | April 2008
Characterization
of impurities
Some of IPCA’s Unique Products*…..
Physical and /or chemical
incompatible drugs
Artesunate + Amodiaquine
Drugs with different biological
half lives
Loratidine + Pseudoephedrine
Multiple release
formulations
Bilayer
Antidiabetic drug combinations
Inlay
Zolpidem tartarte ER
Trilayer
Metformin ER +Glicazide MR + Pioglitizone IR
To prevent side effects
Lamotrigene MR tablets
Mumps – multiple unit particulate
system
Filled in hard gelatin capsule
Compressed within a tablet
(Metoprolol Succinate XL)
*For Indian Market
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Snehal Khedkar | April 2008
The starting formulation may be based on
INTUITION
but the ending formulation must be based on
SCIENCE
Science means: There will be no weak eye in the
pharmaceutical development chain
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Snehal Khedkar | April 2008
Research & Development (Formulations)…..
New Product Introduction
Pharmacology
Evaluation
Regulatory
Affairs
R&D
Analytical
Research
Divisions
Medical
Marketing
Identification
Product
Development
Developm
ent
Evaluation
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Snehal Khedkar | April 2008
R&D
Production
Q.A.
R&D Production
Validation team
Validation
Tech.
Transfer
Regulatory
Development Program Timelines…..
Stages
Months
Activities
4
Pre-formulation
Establish Drug : Excipients
compatibility
3
Development lots
Mini experimental trials to decide the
formula / process
2
Process optimization
Fine tuning to avoid scale-up problem
Process qualification
(Scale-up batch)
To define critical processing steps
and test parameters usually mimics
production conditions
Stability
Studies
Pivotal batch
4
2
Product development
report & Submission
Samples are used to perform the bioequivalence study / clinical trials.
For PAI visit
~ 15 Months for Product Development, by Following ICH Guidelines
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Snehal Khedkar | April 2008
Technology Transfer…..
100
R&D Development
More effective as we move
point of intersection to the left
Manufacturing
& Quality
0 Early Development
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Snehal Khedkar | April 2008
Launch / Commercialization
•
Master Manufacturing Document
•
Development Report
•
Specifications
•
Validation Protocols/SOPs
•
Onsite training & technical Presentation
Product Quality Design…..
Knowledge space
DESIGN SPACE
CONTROL
STRATEGIES
Existing knowledge & new scientific data
generated in the process
Design space
Interaction of input variables & process
parameters that provides Quality Product
Control strategy
Includes Input material controls, Process
controls & FPP control tests
Development of
‘ASSURED QUALITY PRODUCT’
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Snehal Khedkar | April 2008
BECAUSE
Knowledge space & resulting design space & process understanding
CONSTANTLY EVOLVES……!!
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Snehal Khedkar | April 2008