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Caffeine is white, slightly bitter, odorless,

Extraction of Caffeine from Tea

1,3,7-trimethylxanthine (caffeine)

3160
Mail: cwlin@tmu.edu.tw

crystalline solid. mp: 238 oC


Biological action of caffeine:
Central nervous System stimulation
Cardiac stimulation
respiratory stimulation
Diuretic effect
Nervousness
Insomnia
Tachycardia (racing heartbeat)
Caffeinism (more than 600 mg a day) : chronic
insomnia, ringing in the ears (
), persistent
anxiety, stomach upset, and mild delirium (

Caffeine content: 2-4 % (w/w)


The solubility of caffeine in water is
22 mg/mL at 25 oC
180 mg/mL at 80 oC
670 mg/mL at 100 oC.
Caffeine is far more soluble in
Dichloromethane: 10.2 g per 100 mL at 20 oC.
The solvent used in this experiment
to extract the caffeine from water.
extraction rate 30 %

Tea leaves or coffee beans contain:


Caffeine
Cellulose
Plant proteins
Fats
Soluble sugars
Peptides
Chlorophyll pigments
Tannins

Caffeine content of Tea is 50~100 mg/cup


Caffeine content of coffee is 100~200 mg/cup
Chemical constituents of Green tea are
Caffeine 2~4%
Amino acids 4%(theanine 2%)
Lignin 6.5%
Organic acid 1.5%
Protein 15%
Chlorophyll 0.5%
Polyphenols 8~12%

structure of tannins :

Tannins and gallic acid


Na2CO3
CH2Cl2-insoluble sodium salt
caffeine

Na2CO3

No reaction, so
caffeine remains
CH2Cl2 soluble

Techniques used in this experimental:


1. Solid/liquid extraction
Na2CO3

2. Liquid/liquid extraction (gentle)


3. Washing
4. Drying organic solution
5. Removing solvents
6. Emulsion

Washing:
a. 5% NaHCO3, b. Brine

Emulsion

Washing is accomplished by placing


the organic solution in the s. f. along
with the wash solution, then Shaking
and separating in the usual Manner.

A number of techniques are available for


dealing with emulsion

4. Filtering the mixture with vacuum, then


proceeding with separation.
5. Drawing off as much of the lower layer in the s. f.

1. Allowing the s. f. to sit in an iron ring for a few


minutes with gentle swirling.
2. Adding a few drops of a saturated solution of
aqueous sodium chloride with a dropper.
3. Squirting a few drops of 95% ethanol or
commercial antifoam agent on the emulsion bubbles

as possible, adding fresh solvent to the top layer


remaining in the funnel to dilute it, and swirling
gently.
6. Pouring the mixture into a flask, corking the flask,
and allowing the mixture to sit overnight.

Experimental Procedure:
place 6.0g anhydrous Na2CO3 in a beaker

Materials:
1.Tea leaves
2.Cheese clothes
3.Anhydrous Na2CO3
4.CH2Cl2
5.Brine
6.Anhydrous MgSO4

add 100 mL of dist. water


place cheese cloth containing 10 g of tea
leaves
gentle boil for 20 min
cooled
transfer the black soln into s. f.
extract with 20 mL of CH2Cl2 (3X)
CH2Cl2 layer wash with 20 mL of D. W.
CH2Cl2 layer wash with 20 mL of Brine

transfer CH2Cl2 layer into a E.

Caffeine/BS

flask (clean & dry )


add anhydrous MgSO4

CH2Cl2
layer 1

stand for 5 min

Caffeine/BS

gravity filtration (received by a


CH2Cl2
layer 2

Caffeine/BS

CH2Cl2
layer 3

Combined CH2Cl2. Layer


wash with D. W and Brine,
dry (MgSO4), evaporate

BS

Discard

R. B. flask,

remove solvent by Rotary


Evaporator
weigh the crude caffeine

1. Extraction

Basic Techniques
1. Extraction
2. Filtration
3. Using a rotary evaporator

Steps in extraction
1. Preparation of separatory funnel
2. Adding the liquid
3. Mixing the layers
4. Separating the layers
5. Cleaning the separatory funnel
2

1.Preparation of separatory funnel

2. Adding the liquids

Set the s. f. in
an iron ring

Do not fill the


s. f. more than
three-quarters
full

3. Mixing the layers

4. Separating the layers

How to prepare fluted filter paper

2. Filtration:
a. Gravity filtration (simple filtration)

3. Using a rotary evaporator

Steps in using a rotary


evaporator

Cool ice circulator

3. adjust the apparatus so that


the flask containing the
solution is approximately
one-third submerged in a
water bath

1. Select a round-bottomed
flask: half-full or
less with the solution
2. Connect the flask to the
rotary evaporator with
a joint clip

13

12

4. turn on the vacuum source

Capillary feed tube:


1.
:
2.
:

5. turn on the motor that rotates the evaporating


flask
6. heat the water bath (30-40 oC)

when solvent no longer condenses in the


receiving flask, the distillation is complete.
7. stop the rotation of the flask and raise it from
the heating bath
8. open the stopcock and allow air to bleed into
the system
9. hold the flask with one hand and remove the
clip holding it to the evaporator

1. Power on

10. turn off the vacuum source

2. Set temp: 30-40oC

11. Weight the crude extract


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