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INTRODUCTION :-
• Lyophilization is also known as Freeze Drying or Cryodesiccation is a dehydration
process typically used to preserve a perishable material or made the material more
convenient for transport.
• It is a special form of drying that removes all moistures and tends to have less effect on
a food’s taste than normal dehydration process.
• In this process , food is frozen and placed in a strong vacuum . The water in the food
sublimates , it turns straight from ice into vapour.
• Process was first applied to the food products after the second world war.
• Coffee was first freeze dried food product to be produced.
DEFINITION :-
A stabilizing process in which a substance is first frozen and then the quantity of the solvent is
reduced , first by sublimation (primary drying stage) and then desorption (secondary drying
stage) to values that will no longer support biological activity or chemical reactions.
PRINCIPLE :-
• Lyophilization is carried out using a simple principle of physics sublimation. Sublimation
is the transition of a substance from the solid to the vapour state , without first passing
through an intermediate liquid phase.
• Lyophilization is performed at temperature and pressure conditions below the triple
point , to enable sublimation of ice.
• Triple point of water is a point where , water exists in all the three phases, the solid , the
liquid and the gas. This point is achieved at the temperature of 0.01°C and the pressure
of 0.00603 atm.
• The entire process is performed at low temperature and pressure by applying vacuum ,
hence is suited for drying of thermolabile compounds.
• So , when the process is performed below these conditions the solid ice is directly
converted into the gaseous form without converting into the liquid.
• So , in this technique thr liquid is frozen to solid and then is converted to gas , to remove
all the moisture or solvent present in it.
TYPES :-
The types of lyophilizer are classified as –
1. On the basis of their size.
2. On the basis of their capacity.
1. On the basis of size :- Depending upon the size they can be classified as –
A Typical Manifold Dryer
B Shelf Freeze Dryer
C Combination Lab Freeze Dryer
2. On the basis of capacity :- Depending upon the capacity they can be classified as –
A Bench Top Freeze Dryer
B Pivot Freeze Dryer
C Production Freeze Dryer
COMPONENTS OF LYOPHILIZER :-
The main components of lyophilizer are –
• Chamber
• Shelves
• Refrigerator System
• Condenser
• Vacuum Pump
1. Chamber :- A chamber is tight insulated box pf stainless steel consisting of shelves.
2. Shelves :- Shelves on which products are kept and acts as a heat exchanger.
3. Refrigerator System :- A refrigerator system , which has a compressor which cools the
condenser.
4. Condenser :- Condenser is a form of coils or plates for trapping solvent vapours.
5. Vacuum Pump :- A vacuum pump is there for lowering the temperature.
PROCESS OF LYOPHILIZATION :-
The process of lyophilization involves following steps –
1. Pre treatment
2. Freezing Stage
3. Primary Drying Stage
4. Secondary Drying Stage
5. Packing
1. Pre Treatment :-
• This stage include all the methods of treating the product prior to freezing
• Such as – concentrating the product to make it stable such that the minimum amount of
the solvent is present from the beginning only.
• Formulation revision i.e addition of cryoprotectants.
• Decreasing the high vapour pressure solvent.
• Increasing the surface area.
2. Freezing Stage or Freeze Drying Stage :
• In this stage the product is frozen to ice.
• The product is frozen below it’s euthentic temperature.
• Low temperature and pressure is maintained.
• Decreasing the shelf temperature to -50°C.
• In the laboratory , it is done by placing the product in the freeze dryer flask , which is
rotated in the shell freezer bath , which is cooled by dry ice , methanol or mechanical
refrigeration etc.
3. Primary Drying [ Sublimation ]:
▪ In the stage the temperature and pressure are kept below the triple point of water .
▪ That is the temperature.0.0098°C and pressure 4.58 mmHg
▪ Heat is introduced from the shelf to the product under the granted control by electrical
resistance cells or circulating silicon.
▪ Rate of sublimation of ice depends upon difference in V.P of product ad V.P of
condenser
▪ 95-98% of Water is removed , and process takes 20-24 hours .
4. Secondary Drying [ Desorption ]:
▪ It is also known as Isothermal Desorption
▪ Which removes the remaining solvent form the product .
▪ It removes the bound water .
▪ It is continued at same pressure but the temperature is increased around +10-40°C
▪ It takes about 10-20hrs.
5. Packing :
▪ After drying the vaccum is replaced by filtered air or nitrogen to establish atmospheric
pressure .
▪ Ampoules are sealed by either tip sealing or clousers and aluminium caps .
▪ Vials and bottles are sealed with rubber clousers and alluminium caps.
APPLICATIONS OF LYOPHILIZATION :-
Following are the applications of lyophilization –
1. Pharmaceutical Industry and Biotechnology :-
• Pharmaceutical companies often use freeze drying to increase the shelf life of products ,
such as vaccines and other injectable.
• By removing the water from the material and sealing the material in a vial , the material
can be easily stored , shipped and later reconstituted to its original form for injection.
2. Food Industry :-
• Freeze – drying is used to preserve food and make it very light weight.
• The process has been popularized in the forms of freeze dried icecream ; an example of
astronaut food.
• Instant coffee powder is prepared.
• To produce essences or flavouring agents.
• Culinary herbs are preserved.
• Freeze dried fruits are produced.
3. Technological Industries :-
• In chemical synthesis , products are often lyophilized to make them more stable , or
easier to dissolve in water for subsequent use.
• It is also capable of concentrating substances with low molecular weights that are two
small to be removed by a filtration membrane.
4. Other uses :-
• Freeze-drying is used for flora and fauna preservation.
• It is also used for recovery of water- damaged books and documents.
ADVANTAGES OF LYOPHILIZATION :-
Following are the advantages of lyophilization –
• Minimum damage to heat labile material.
• Removal of water at low temperature.
• Compatible with aseptic operations.
• Sterility can be maintained.
• Reconstitution is easy.
• Increasing shelf life of the product.
• Doesnot shrink the samples.
• Reduces weight and volume of samples ; ideal for shipping .
• Samples can be stored at room temperature indefinitely.
DISADVANTAGES OF LYOPHILIZATION :-
Following are the disadvantages of lyophilization –
• High capital cost of equipment.
• High energy cost.
• Time consuming process ( Typically 4-10 hrs per drying cycle ).
• Possible damage to products due to change in pH and tonicity.
• Many biological molecules are damaged by the stress associated with freezing.
• The open porous structure of the food may allow oxygen to enter and cause oxidative
degradation of lipids (packing in inert gas necessary).

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Lyophilizationn.pdf

  • 1. INTRODUCTION :- • Lyophilization is also known as Freeze Drying or Cryodesiccation is a dehydration process typically used to preserve a perishable material or made the material more convenient for transport. • It is a special form of drying that removes all moistures and tends to have less effect on a food’s taste than normal dehydration process. • In this process , food is frozen and placed in a strong vacuum . The water in the food sublimates , it turns straight from ice into vapour. • Process was first applied to the food products after the second world war. • Coffee was first freeze dried food product to be produced. DEFINITION :- A stabilizing process in which a substance is first frozen and then the quantity of the solvent is reduced , first by sublimation (primary drying stage) and then desorption (secondary drying stage) to values that will no longer support biological activity or chemical reactions. PRINCIPLE :- • Lyophilization is carried out using a simple principle of physics sublimation. Sublimation is the transition of a substance from the solid to the vapour state , without first passing through an intermediate liquid phase. • Lyophilization is performed at temperature and pressure conditions below the triple point , to enable sublimation of ice. • Triple point of water is a point where , water exists in all the three phases, the solid , the liquid and the gas. This point is achieved at the temperature of 0.01°C and the pressure of 0.00603 atm. • The entire process is performed at low temperature and pressure by applying vacuum , hence is suited for drying of thermolabile compounds. • So , when the process is performed below these conditions the solid ice is directly converted into the gaseous form without converting into the liquid. • So , in this technique thr liquid is frozen to solid and then is converted to gas , to remove all the moisture or solvent present in it.
  • 2. TYPES :- The types of lyophilizer are classified as – 1. On the basis of their size. 2. On the basis of their capacity. 1. On the basis of size :- Depending upon the size they can be classified as – A Typical Manifold Dryer B Shelf Freeze Dryer C Combination Lab Freeze Dryer 2. On the basis of capacity :- Depending upon the capacity they can be classified as – A Bench Top Freeze Dryer B Pivot Freeze Dryer C Production Freeze Dryer COMPONENTS OF LYOPHILIZER :- The main components of lyophilizer are – • Chamber • Shelves • Refrigerator System • Condenser • Vacuum Pump
  • 3. 1. Chamber :- A chamber is tight insulated box pf stainless steel consisting of shelves. 2. Shelves :- Shelves on which products are kept and acts as a heat exchanger. 3. Refrigerator System :- A refrigerator system , which has a compressor which cools the condenser. 4. Condenser :- Condenser is a form of coils or plates for trapping solvent vapours. 5. Vacuum Pump :- A vacuum pump is there for lowering the temperature. PROCESS OF LYOPHILIZATION :- The process of lyophilization involves following steps – 1. Pre treatment 2. Freezing Stage 3. Primary Drying Stage 4. Secondary Drying Stage 5. Packing
  • 4. 1. Pre Treatment :- • This stage include all the methods of treating the product prior to freezing • Such as – concentrating the product to make it stable such that the minimum amount of the solvent is present from the beginning only. • Formulation revision i.e addition of cryoprotectants. • Decreasing the high vapour pressure solvent. • Increasing the surface area. 2. Freezing Stage or Freeze Drying Stage : • In this stage the product is frozen to ice. • The product is frozen below it’s euthentic temperature. • Low temperature and pressure is maintained. • Decreasing the shelf temperature to -50°C. • In the laboratory , it is done by placing the product in the freeze dryer flask , which is rotated in the shell freezer bath , which is cooled by dry ice , methanol or mechanical refrigeration etc. 3. Primary Drying [ Sublimation ]: ▪ In the stage the temperature and pressure are kept below the triple point of water . ▪ That is the temperature.0.0098°C and pressure 4.58 mmHg ▪ Heat is introduced from the shelf to the product under the granted control by electrical resistance cells or circulating silicon. ▪ Rate of sublimation of ice depends upon difference in V.P of product ad V.P of condenser ▪ 95-98% of Water is removed , and process takes 20-24 hours . 4. Secondary Drying [ Desorption ]: ▪ It is also known as Isothermal Desorption ▪ Which removes the remaining solvent form the product . ▪ It removes the bound water . ▪ It is continued at same pressure but the temperature is increased around +10-40°C ▪ It takes about 10-20hrs.
  • 5. 5. Packing : ▪ After drying the vaccum is replaced by filtered air or nitrogen to establish atmospheric pressure . ▪ Ampoules are sealed by either tip sealing or clousers and aluminium caps . ▪ Vials and bottles are sealed with rubber clousers and alluminium caps. APPLICATIONS OF LYOPHILIZATION :- Following are the applications of lyophilization – 1. Pharmaceutical Industry and Biotechnology :- • Pharmaceutical companies often use freeze drying to increase the shelf life of products , such as vaccines and other injectable. • By removing the water from the material and sealing the material in a vial , the material can be easily stored , shipped and later reconstituted to its original form for injection. 2. Food Industry :- • Freeze – drying is used to preserve food and make it very light weight. • The process has been popularized in the forms of freeze dried icecream ; an example of astronaut food. • Instant coffee powder is prepared. • To produce essences or flavouring agents. • Culinary herbs are preserved. • Freeze dried fruits are produced. 3. Technological Industries :- • In chemical synthesis , products are often lyophilized to make them more stable , or easier to dissolve in water for subsequent use. • It is also capable of concentrating substances with low molecular weights that are two small to be removed by a filtration membrane. 4. Other uses :- • Freeze-drying is used for flora and fauna preservation. • It is also used for recovery of water- damaged books and documents.
  • 6. ADVANTAGES OF LYOPHILIZATION :- Following are the advantages of lyophilization – • Minimum damage to heat labile material. • Removal of water at low temperature. • Compatible with aseptic operations. • Sterility can be maintained. • Reconstitution is easy. • Increasing shelf life of the product. • Doesnot shrink the samples. • Reduces weight and volume of samples ; ideal for shipping . • Samples can be stored at room temperature indefinitely. DISADVANTAGES OF LYOPHILIZATION :- Following are the disadvantages of lyophilization – • High capital cost of equipment. • High energy cost. • Time consuming process ( Typically 4-10 hrs per drying cycle ). • Possible damage to products due to change in pH and tonicity. • Many biological molecules are damaged by the stress associated with freezing. • The open porous structure of the food may allow oxygen to enter and cause oxidative degradation of lipids (packing in inert gas necessary).