#FreezeDryer

1. GURU NANAK INSTITUTE OF
PHARMACEUTICAL SCIENCE AND
TECHNOLOGY
Presented by- Jinia Rina Ghosh(18601919065)
Kaenat Faiz(18601919068)
Ayan Sarkar(18601919072)
Ahana Paul(18601919076)
Piyali Basak(18601919088)

2. CONTENTS
 Introduction
 Principle
 Construction
 Working
 Advantages and Disadvantages
 Applications of freeze drying
 Desired characteristics of freeze dried products
 Practical aspects of freeze drying
 Maintenance
 Conclusion
 Reference

3. INTRODUCTION
Drying:
 Drying is an important technique used in industry.
Prevent deterioration.
 Improves solubility.
 Removes trace amount of water or liquid by heat.
Equipments for drying:
 Tray dryer
 Spray dryer
 Fluid bed dryer
 Vacuum dryer
 Drum dryer
 Freeze dryer
Freeze Drying:
 Lyophilisation
 Material is freeze then high pressure vacuum is applied
 First applied in food products.
 Most common unit process for manufacturing drug products too unstable to be marketed as solutions.
 Instrument used for freeze drying, is called freeze dryer.
[1]

4. PRINCIPLE
Water is removed from the
frozen state sublimation.
Drying is achieved by subjecting
material below freeing point.
Under these condition any heat
transferred is used as latent heat
and ice sublimes directly into
vapor state.
[1]

5. CONSTRUCTION
Chamber
Process Condenser
Shelf Fluid
Refrigeration centre
Vacuum system
Control system
[2]

7. WORKING
• Volume of
solution is
limited by its
capacity.
• Pretreatment
• Solution is
pre-
concentrated
Preparation &
Pretreatment
• Vials,
ampoules,
bottles in
which the
solution is
packed are
frozen.
• Cabinet is
maintained
at low
temperature
and pressure
Freezing
• Temperature
and pressure
is below
triple point
• Vacuum is
applied
• Temperature
is increased
linearly
• Ice sublimes
into vapor
• Vapor is
moved to the
condenser.
Primary
Drying
• Traces of
moisture is
removed but
temperature
of solid of
solid is raised
to as 50-
60°C.
• But vacuum
is lowered
below that is
used in
primary
drying.
Secondary
Drying • The final
product is
packed.
• Vial-sealing
• Defrost
• CIP
• SIP
• H2O2
Packing
[2]

10. Fig: Lyophilisation process
Fig: Example of freeze-drying

11. ADVANTAGES
1. Thermolabile materials can be dried.
2. Denaturation does not occur.
3. Loss of volatile material is less.
4. Sterility can be maintained.
5. Material can be dried in its final container
such as single does and multiple dose vials.
6. No need to refrigerate.
7. Less damage to the physical structures.
8. Constituents of the dried material remain
homogenously dispersed.
DISADVANTAGES
1. Expensive.
2. Time-consuming process.
3.Effective for selected items.
4. Difficult for solutions containing non-aqueous
solvents.
5. Some issues associated with aseptic loading of
vials into the chamber.
6. Volatile compounds may be removed by high
vacuum.
[2] [2]

12. APPLICATIONS OF FREEZE DRYING
Industry Applications
1. Ceramics To create formable powder.
2. Pharmaceuticals Proteins, vaccines, enzymes, hormones
etc.
3. Food processing Flavorings, juices, instant meals and soups
etc.
4. Dairy industry High value proteins.
5. Technological
Industry
Chemically synthesized products, late
stage purification procedures.
6. Research Stabilization and storage of biological
materials.
Fig: Food processing
Fig: Ceramics
Fig: pharmaceuticals
[2,3]

13. DESIRED CHARACTERISTICS OF FREEZE DRIED
PRODUCTS
 Intact cake
 Sufficient strength
 Uniform color
 Sufficiently dry
 Sufficiently porous
 Sterile
 Free of pyrogens
 Free of particulates
 Chemically stable
Fig: Freeze-dried ice-cream
Fig: Freeze-dried fruits
Fig: Freeze-dried sterile
pharmaceutical products
[2]

14. PRACTICALASPECTS OF FREEZE-DRYING
• Have appropriate analytical tools and methods in place for formulation characterization and stability
studies.
• Depend on literature, previous experience (if none, use consultants).
• Initial formulations should use commonly-known excipients used in freeze-drying.
• Solids content should be between 5% and 30% with a target of 10% to 15%.
• Should have several initial formulations to evaluate and compare.
• Determine appropriate processing parameters.
• Optimize formulation and process based on stability information.
[3]

15. MAINTENANCE
• Freeze dryer PC maintenance when the system is running slow.
• Freeze dryer vacuum pumps maintenance.
• Refrigeration should be checked by functional tests every four months.
• Cleaning and calibration
• The condenser temperature should be 10 to 15°C below the sample’s eutectic point.
• Certain acids should not be used with bare stainless steel and should only be used with
PTFE models.
• Defrost and drain the condenser after each standard run.
• Neutralize the chamber if acid is being used.
• Do not overload freeze dryer.
• Put completely frozen sample.
[2]

16. CONCLUSION
 Freeze drying or lyophilization is process in which water is frozen, followed
by its removal from a sample, initially by sublimation, then by desorption.
 The term lyophilisation describes a process to produce a product that loves the
dry state.
 This is applicable in various pharmaceuticals, food industry, for thermolabile
products, substances that are unstable in aqueous solutions etc.
 Maintaining all the steps uniformly, all the desired products can be obtained
ensuring the maximum productivity.
[1]

17. REFERENCE
1. Lachman. L.; Liberman. H.A. Joseph.B.S. Pharmaceutical
dosage form tablet.2,Marcell Dekker Vol.1 126-137
2. Remington. The science and practice of Pharmacy 20.
Lipincott William and winkins. Vol.1 525-532
3. Martin. A.; Physical
Pharmacy.4,B.I.Warly.pvt.ltd.NewDelhi.22-40
4. GEA Pharma & Healthcare - https://youtu.be/9iS0usklM58