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CAFFEINE EXTRACTION AND CHARACTERIZATION

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 Research Article
CAFFEINE EXTRACTION AND
CHARACTERIZATION
IJCRR
Section: General
Science
Sci. Journal Pradeep S.1, G. N. Rameshaiah2, Hadagali Ashoka1
Impact Factor
4.016
Department of Biotechnology, 2Department of Chemical Engineering BMS College of Engineering, Bull Temple Road, Bangalore- 560019,
1

Karnataka, India.

ABSTRACT
Caffeineextracted and characterised from tea (black) leaves and coffee beans. Isolation was done by liquid-liquid extraction us-
ing di-chloromethane as an extracting agent. This extraction was done in four steps: steeping, evaporation, liquid-liquid extrac-
tion and recrystallization. The recrystallization was done using anhydrous sodium sulphate.The technique used for purity analy-
sis and characterisation were: High performance liquid chromatography, Differential scanning calorimeter, Fourier transform
infrared spectroscopyand Melting point. First, the analysis was done using melting point analysis. The melting point of caffeine
extracted from coffee beans and tea leaves was found to be 238°C. The absorption bands were compared with that available
in literature and were found to be similar. Further, the purity check was done using High performance liquid chromatography
method.Effective characterization of caffeine was achieved by determining Infrared spectrum, and employing a melting point ap-
paratus and differential scanning calorimeter. The purity showed that the results that the extracted coffee was 90% pure. Further
improvements in extraction efficiency will increase the yield and minimize wastage.
Key Words: Caffeine, Methyl xanthine, Theophylline, Differential scanning calorimeter, Fourier transform infrared spectroscopy,
High performance liquid chromatography

INTRODUCTION 3. To develop an easily adaptable method for the qualita-

Caffeine is a psychoactive CNS stimulant drug discovered
by German chemist Friedrich Ferdinand Runge in 1819.
He coined the term ‘Kaffein’ which became Caffeine5.Caf-
feine is a methyl xanthine along with theophylline and
theobromine.It is a natural pesticide.Caffeine does not
counteract the effects of alcohol. Caffeine is a xanthine
alkaloid compound that acts as a stimulant in humans. It
is a central nervous stimulant, having the effect of tem-
porarily warding off drowsiness and restoring alertness.2
Every time we drink tea, coffee, cocoa, chocolate or cola
we are giving our body a “hit” of caffeine. Along with
nicotine and alcohol, caffeine is one of the three most
widely used mood – affecting drugs in the world5.
tive or purity analysis of caffeine
PHYSICAL AND CHEMICAL PROPERTIES
Caffeine is sparingly soluble in most polar solvents but
is highly soluble in less polar solvents. The melting point
is 234°C-239°C and the chemical formula is C8H10N4O2 .It
is an intensely bitter, white powder in its pure state. Caf-
feine is an alkaloid of the methylxanthine family, which
also includes the similar compounds theophylline and
theobromine2.The structure of caffeine is

OBJECTIVES
1. To extract caffeine from tea leaves and coffee beans by
liquid-liquid extraction method. ADMET OF CAFFEINE
2. To characterize the obtained caffeine by melting
Absorption & Distribution
point, Infrared spectroscopy and Differential scanning
Caffeine is absorbed orally with a max blood peak af-
calorimetermethod.
ter 120 mins spreading quickly in all tissues.Caffeine is

Corresponding Author:
Corresponding Author: of Biotechnology BMS College of Engineering, Bull Temple Road, Bangalore- 560019, Karnataka, India
Pradeep S., Department
Anil Pawar, Assistant Professor, Department of Zoology, D.A.V. College for Girls, Yamunanagar (Haryana); Mobile:919467604205;
E-mail: padees@gmail.com
Email: sumanil27@yahoo.co.in
Received: 13.02.2015 Revised: 11.03.2015 Accepted: 10.04.2015
Received: 16.6.2014 Revised: 11.7.2014 Accepted: 29.7.2014

Int J Cur Res Rev | Vol 7 • Issue 9 • May 2015 16

 Pradeep et. al.: Caffeine Extraction and Characterization

classified as a stimulant because it increases the activ-
ity of cardiovascular, digestive and sympathetic nervous
system, and produces the sense of alertness in the brain.
It can have a lethal effect ( acute intoxication) when in-
gested at amounts of 1-5 g, with plasma concentrations
higher than 80mg/ml and the first intoxication signs ap-
pear at about 250mg4.
Metabolism and Elimination
Hepatic metabolism becomes longer and more difficult
in presence of alcohol and medical drugs while cigarette
smoke accelerates its hepatic metabolism.Only 10% is
eliminated through the kidney as unmodified caffeine4.
ride, anhydrous sodium sulphate, Whatmann no.1 filter
paper,15ml of dichloromethane,50ml and 500ml of Er-
lenmeyer flask, separating funnels, MilliQwater,etc.
CHARACTERIZATION OF CAFFEINE
Based on various physical methods.
1.  Determination of melting point
2.  Infrared spectroscopy
3.  Degradation by Differential scanning calorimeter

4.  Purity check by High performance liquid chromatog-

Caffeine intoxication raphy
The symptoms include restlessness, nervousness, and ex-
citement, insomnia, flushing of the face, increased urina-
tion, gastro-intestinal disturbance, muscle twitching, and RESULTS
psychomotor agitation.The treatment is based on serum
levels of caffeine which may be followed by peritoneal Extraction of caffeine from tea and coffee was achieved
dialysis, hemodialysis, or hemo filtration. Caffeine stimu- by using chloroform as an extracting solvent.
lates acid production in the stomach so it is better not to
drink coffee in case of gastric ulcer4 Table 2: Isolation and purification of caffeine from
tea and coffee
Sl.no Sample Amt of Amt of caffeine after
Table 1: Caffeine content of selected common food
sample(g) solvent extraction(g)
and drug products.
1. Tea 5 0.167
Sl. No. Product Serving size Caffeine/serving
in mg 2. Coffee 5 0.252

1. Caffeine One tablet 200 Table 3: Characteristic Infrared- Absorption bands of

tablet sample and standard
2. Chocolate One bar(43g) 31 Sl.no Bonds Standard Tea Coffee
3. Soft drinks 350ml 34 1. C-H 2955.23 2955.50 2956.25
2. C=C 1550.03 1550.57 1550.25
3. C=O 1701.30 1701.96 1701.41
EXTRACTION OF CAFFEINE
4. C-N 1239.95 1240.18 1240.49
Steeping procedure is used.The solvent used is dichlo- 5. C=N 1660.77 1661.25 1661.89
romethane.Purification methods like distillation and
recrystallization are also followed.The success of extrac- Table 4: Characteristics of purified caffeine isolated
tion involving a natural product is often expressed as from tea and coffee
percentage recovery. Sl. Sample Melting point Average
Grams of caffeine recovered no
% recovery =
1. Standard 238.25 238.15 238.25 238.2
Grams of tea leaves
2. Tea 237.45 237.5 237.85 237.6
The percentage recovery is called the purified percent 3. coffee 237.85 237.95 238.55 238.11
recoveryor crude percent recovery. The extraction with
the highest percent recovery is considered the most suc- Table 5: Differential scanning calorimeter
cessful extraction5.
Sl.no Sample Degradation point
1. Standard 237.41
MATERIALS REQUIRED 2. Tea 237.69
5g of tea leaves, 10g coffee beans, 4g of calcium car- 3. Coffee 237.45
bonate, 2g sodium carbonate, 25ml methylene chlo-

17 Int J Cur Res Rev | Vol 7 • Issue 9 • May 2015

 Pradeep et. al.: Caffeine Extraction and Characterization

Table 6: Caffeine determination in green tea, black

tea and coffee. (byHigh performance liquid chroma-
tography )
Sl. Sample RT(mins) Area Height Area%
no
1. Standard 12.13 8541.18 548.12 99.96
2. Tea 12.14 7348.59 471.26 89.75
3. Coffee 12.15 7406.75 483.39 89.62

Figure 3: Differential scanning calorimeter reading of caffeine

samples

Figure 1: Melting point reading.

Figure 4: Peak areas of caffeine sample obtained through

newly adapted High performance liquid chromatography meth-
od.

Figure 2: Fourier transform infrared spectroscopy spectrum of
caffeine sample
DISCUSSION
It was observed that the extraction efficiency of caffeine
from various sources by using chloroform was much
higher than other solvents. Table 2 shows the extraction
efficiency of crude caffeine from tea and coffee leaves.
The amount of caffeine obtained from L- L extraction af-
ter further recrystallization was found to be 3.37% from
tea and 5.04% from coffee.We observed that coffee con-
tained a high percentage of crude caffeine as compared
to tea. To purify the crude caffeine, similar procedures
were utilized.

However, the caffeine content of various sources varies

with soil conditions and climate. Table 3-6 shows the
characteristics of caffeine in various parameters for both
sample and standard respectively. Also 2-5 shows the re-
sult of caffeine samples being measured respectively.

The pure white crystalline caffeine isolated from sources

was found to melt at 238oC. The Infrared-spectrum of
isolated caffeine showed similar absorption bands simi-
lar to that given in literature. The Infrared-spectrum in-
dicates the absolute purity of the purified caffeine.

Int J Cur Res Rev | Vol 7 • Issue 9 • May 2015 18

 Pradeep et. al.: Caffeine Extraction and Characterization
We have developed a High performance liquid chro-
matography method for the determination of caffeine,
which was carried by High Performance Liquid Chroma-
tography instead of using UV- Visible spectrophotometer.
We chose High performance liquid chromatography
method for the determination of caffeine, because High
performance liquid chromatography is the most widely
used qualitative and quantitative determination and
separation method. This method is popular because it
is non-destructive and unlike gas chromatography may
be applied to thermally liable compounds. Moreover it is
also a very sensitive technique as it incorporates a wide
range of detection methods. With the use of post column
derivatization methods to improve selectivity and detec-
tion limits, High performance liquid chromatography can
easily be extended to trace determination of compounds
that do not usually provide adequate detector response.
The wide applicability of High performance liquid chro-
matography as a separation method makes it a valuable
separation tool in many scientific fields.
By using this method, we determined the retention time
and the relative peak area of extracted purified caffeine.
The retention time of the purified caffeine and that of the
standard caffeine were almost similar, which confirmed
the identity of caffeine. The amount of extracted purified
caffeine for different samples was determined by study-
ing the relative peak area on the calibration curve.
CONCLUSION
A method has been developed for the extraction, puri-
fication of caffeine from tea and coffee. Caffeine from
tea and coffee was extracted by liquid- liquid extraction
followed by recrystallization. The purified caffeine was
then analysed by High performance liquid chromatogra-
phy. Effective characterization of caffeine was achieved
by determining IR spectrum, and employing a melting
point apparatus and differential scanning calorimeter.
19
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The serious concern about potential use of caffeine for
pathogenic effects has made it one of the most broadly
studied drugs. It provides clinicians with the information
they require in order to understand, diagnose and treat
the effects of caffeine consumption in their patients.
ACKNOWLEDGEMENT
Authors acknowledge the immense help received from
the scholars whose articles are cited and included in ref-
erences of this manuscript. Authors are also grateful to
authors, editors and publishers of all those articles, jour-
nals and books from where the literature for this article
has been reviewed and discussed.
REFERENCES
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Int J Cur Res Rev | Vol 7 • Issue 9 • May 2015