This document summarizes research on optimizing the yield of cinnamon essential oil extraction using microwave-assisted extraction. The objectives were to extract cinnamon oil using microwave extraction and optimize parameters to maximize yield. Experimental work involved extracting oil from cinnamon powder using microwave extraction at different solid loadings, solvent quantities, microwave power levels, and extraction times. Analysis found the optimum conditions were 35g solid loading, 250ml solvent, 700W power for 30 minutes, yielding 4.837% oil. Microwave extraction yielded more oil faster than hydrodistillation and was more efficient.

1. Optimization of yield for extraction of an
essential oil from Cinnamon using
Microwave-assisted extraction
Prepared by : SatishKumar K. Movaliya
Enrollment no. : 150170730008
Guided by : Prof. Yogesh J. Morabiya
Vishwakarma Government Engineering College, Chandkheda
Ahmedabad-382424
31st May, 2017

2. Outlines
Research Objectives
Introduction
Microwave-assisted extraction
Research gap from literature survey
Experimental work
Design of Experiment (DOE)
Results
Conclusion
Future scope of work
References

3. To extract an essential oil from cinnamon by using novel technique –
Microwave assisted extraction and Optimization of Microwave
extraction process parameter to obtain maximum yield of cinnamon
oil.
To analyze the components which are present in essential oil by GC-
MS.
Comparison of novel techniques with hydrodistillation and find out the
predictive model by using ANN (Artificial neural network).
Research objectives

4.  Properties of cinnamon oil
 Scientific name : Cinnamomum verum, Cinnamomum cassia, Cinnamomum
zeylanicum, Cinnamomum loureirii
 Common name : Cinnamon, Cinnamomon, Ceylon cinnamon, Chinese cinnamon,
Chinese cassia, Saigon cinnamon
 Molecular formula : C9H8O
 Molecular weight : 132.383 g/mol
 IUPAC name : 2-methoxy-4-prop-2-enylphenol
 Solubility : Soluble in 1-2.5 vols of 70% alcohol
 Specific gravity : 1.020-1.030 at 20°C
 Refractive index : 1.568-1.535 at 20°C
Introduction

5.  Cinnamon
Introduction
Structure of cinnamon oil [67]Cinnamon sticks, powder and dried flowers [67]

6.  Principle of microwave heating [65]
Microwave-assisted extraction

7. Microwave irradiation effect [65]
Microwave-assisted extraction
Before After

8. Representation of two heating modes : [31]
Microwave-assisted extraction

9.  Important parameters in MAE
 Selection of Solvent
 Solvent-to-Feed Ratio (S/F)
 Extraction time and cycle
 Microwave power level
 Extraction temperature
 Stirring
Microwave-assisted extraction

10. Selection of solvents [65]
Microwave-assisted extraction
Solvent name
Dielectric
constant
Boiling point (°C) Viscosity (cP)
Acetone 20.7 56 0.30
Ethanol 24.3 78 0.69
Hexane 1.89 69 0.30
Methanol 32.6 65 0.54
2-Propanol 19.9 82 0.30
Water 78.3 100 0.89
Ethyl acetate 6.02 77 0.43

11. Research scholars or authors was used only HD and
SCFE for extraction of cinnamon oil
Optimization method not applied
Not use water as a solvent
Research gap from literature survey

12.  Plant material
 1 kg Cinnamon bark collected
Pre-treatment procedure
 Washed into distilled water
 Dried in open air for 1 day at temp. about 25-30°C
 After drying Cinnamon crushed and grinded
 After grinding Cinnamon powder was sieved by mechanical sieve
shaker
 Collect the Cinnamon powder which average particle size was less
than 100 μm
Experimental work

13.  Experimental setup
Experimental work
 RAGA’s Microwave system
 20 liter capacity
 Maximum output power : 700 W
 Input power source : 250 V – 50 Hz
 Microwave frequency : 2450 MHz
 Cavity dimensions : 306 × 𝟐𝟏𝟏 × 320
mm
 Microwave power level :
140 W (20%) 210 W (30%)
240 W (35%) 280 W (40%)
350 W (50%) 420 W (60%)
450 W (65%) 490 W (70%)
560 W (80%) 700 W (100%)

14.  Taguchi method
o Developed by Genichi taguchi
o It is a statistical method sometime called as Robust design method
o Employed this method for improve products or manufacturing processes
o Powerful and effective method to solve challenging quality problems
o Depending upon objectives three norms of mean square deviation
1. Nominal the better
2. Smaller the better
3. Larger the better
Design of Experiment (DOE)

15.  Factors and their levels
Design of Experiment (DOE)
Factors
Levels
1 2 3 4
A Solid loading (gm) 20 25 30 35
B Solvent quantity (ml) 200 250 300 350
C
Microwave power level
(W)
280 420 490 700
D Extraction time (min) 15 20 25 30

16. Design of Experiment (DOE)
Run A B C D
Solid
loading
(gm)
Solvent
quantity
(ml)
Microwave
power level
(W)
Extraction
time (min)
1 1 1 1 1 20 200 280 15
2 1 2 2 2 20 250 420 20
3 1 3 3 3 20 300 490 25
4 1 4 4 4 20 350 700 30
5 2 1 2 3 25 200 420 25
6 2 2 1 4 25 250 280 30
7 2 3 4 1 25 300 700 15
8 2 4 3 2 25 350 490 20
9 3 1 3 4 30 200 490 30
10 3 2 4 3 30 250 700 25
11 3 3 1 2 30 300 280 20
12 3 4 2 1 30 350 420 15
13 4 1 4 2 35 200 700 20
14 4 2 3 1 35 250 490 15
15 4 3 2 4 35 300 420 30
16 4 4 1 3 35 350 280 25

17. Results
Experimen
t no.
Solid loading
(gm)
Solvent
quantity
(ml)
Microwave
power level
(W)
Extraction
time (min)
Yield
(%, w/w)
1 20 200 280 15 2.741
2 20 250 420 20 2.416
3 20 300 490 25 2.395
4 20 350 700 30 3.516
5 25 200 420 25 2.826
6 25 250 280 30 2.734
7 25 300 700 15 3.163
8 25 350 490 20 3.194
9 30 200 490 30 3.558
10 30 250 700 25 4.169
11 30 300 280 20 2.892
12 30 350 420 15 3.159
13 35 200 700 20 4.056
14 35 250 490 15 3.318
15 35 300 420 30 3.449
16 35 350 280 25 2.817

18.  Parametric study
Results

19.  Parametric study
Results

20.  Parametric study
Results

21.  Parametric study
Results

22. Fourier transform infrared spectroscopy (FTIR)
Results

23. Fourier transform infrared spectroscopy (FTIR)
Sample : Cinnamon powder before extraction
Results
Sr. no Wavenumber (cm-1) Functional group names
1 1004 Esters
2 1235 Ethers
3 1431 Nitro group
4 1555 Nitro group
5 1612 Alkenes, Amides, Amines
6 1654 Ketone, Esters, Alkenes
7 2924 Alkanes
8 3261 Alkynes, Phenols, Hydrogen O-H bonded
9 3732 Amines (Primary), Phenol

24. Fourier transform infrared spectroscopy (FTIR)
Results

25.  Fourier transform infrared spectroscopy (FTIR)
Sample : Cinnamon powder after extraction
Results
Sr. no Wavenumber (cm-1) Functional group names
1 1026 Esters, Ethers
2 1089 Ethers
3 1613 Alkenes
4 3369 Carboxylic acids, Phenols

26. Gas chromatography–mass spectrometry (GC–MS)
Results

27.  Gas chromatography–mass spectrometry (GC–MS)
Results
Probable Compound Retention time (min) Area (%)
𝛽-Methyl benzenepropanal 17.818 0.308
Cinnamaldehyde 21.644 89.324
Copaene 24.869 0.807
Coumarin 27.611 0.675
(𝜀)-Cinnamyl acetate 28.002 0.273
𝛾 −Cadinene 29.177 0.325
𝛼 −Muurolene 30.236 1.569
𝛿 −Cadinene 31.236 2.950
𝛼 −Cadinene 31.653 2.225
Cadinadiene-1,4 35.373 0.404
𝛼 −Amorphene 35.933 0.761
𝛼 −Cadinol 36.094 0.383

28. ANOVA (Analysis of variance) Results
Results

29. ANOVA (Analysis of variance) Results
Results

30.  ANN (Artificial neural network)
Results

31.  Coefficient of Regression
for ANN in case of 7 hidden
neurons, FFBP algorithm and
log sigmoid transfer function
Results
R^2 = 99.527
%

32.  Final model equation
Yield = 2.37 + [ 0.433 X1 – 0.00905 X2 – 0.00805 X3 – 0.3244 X4 – 000869 X1^2 +
0.00297 X4^2 + 0.000225 X1*X3 + 0.000463 X2*X4 + 0.000182 X3*X4
Where,
X1 : Solid loading (gm)
X2 : Solvent quantity (ml)
X3 : Microwave power level (W)
X4 : Extraction time (min)
Results

33.  Optimum yield from predictive model by using ANN
Results
Solid Loading (gm) 35
Solvent quantity (ml) 250
Microwave power level (W) 700
Extraction time (min) 30
Predictive yield (%,w/w) 4.837
Actual yield (%,w/w) 4.814

34.  Hydrodistillation method results
Results
Experiment
no.
Solid loading
(gm)
Solvent
quantity (ml)
Extraction
time (min)
Yield
(%, w/w)
1
30 250
30 1.093
2 60 1.472
3 90 1.952
4 120 2.513
5 150 2.806
6 180 3.108

35.  Gas chromatography–mass spectrometry (GC–MS)
Results
Probable Compound Retention time (min) Area (%)
Benzaldehyde 18.916 2.207
Borneol 20.584 1.529
Cinnamaldehyde 23.047 62.60
Coumarin 26.087 1.298
𝛽-Cadinene 29.475 5.204
Trans-𝛼-Bengamotene 29.975 5.847
Camphor 30.236 3.742
𝛼-Humulene 31.380 2.950
Eugerol 32.065 4.603
Guaiacol 32.904 0.865
𝛼-Terpineol 34.237 3.507
Cubenol 34.564 5.602

36. Results
Collected oil

37.  Comparison of MAE with HD
Results
Parameter MAE HD
Solid loading (gm) 30 30
Solvent quantity (ml) 250 250
Microwave power level (W) 700 -
Extraction time (min) 30 180
Maximum yield (%, w/w) 4.169 3.108

38. Microwave-assisted extraction is a rapid extraction technique for
extraction of an essential oil.
In MAE method optimum conditions were obtained at solid loading 35
gm, solvent quantity 250 ml, microwave power level 700 W and
extraction time 30 min.
Microwave power level is more significant parameter for rapid
extraction.
MAE is more cost effective and environmental friendly technique.
Conclusion

39. To study the various properties of cinnamon oil
I. Anti-oxidant activity
II. Anti-microbial activity
III. Zone of inhibition
Future scope of work

40. 1. Y. Li, D. Kong, and H. Wu, “Analysis and evaluation of essential oil components of
cinnamon barks using GC–MS and FTIR spectroscopy,” Industrial Crops and
Products, vol. 41, pp. 269–278, Jan. 2013.
2. R. Li, Y. Wang, Z.-T. Jiang, and S. Jiang, “Chemical Composition of the Essential
Oils of Cinnamomum loureirii Nees. From China Obtained by Hydrodistillation
and Microwave-assisted Hydrodistillation,” Journal of Essential Oil Research, vol.
22, no. 2, pp. 129–131, Mar. 2010.
3. E. Schmidt et al., “Composition and antioxidant activities of the essential oil of
cinnamon (Cinnamomum zeylanicum Blume) leaves from Sri Lanka,” Journal of
Essential Oil Bearing Plants, vol. 9, no. 2, pp. 170–182, 2006.
4. N. Jeyaratnam, A. H. Nour, R. Kanthasamy, A. H. Nour, A. R. Yuvaraj, and J. O.
Akindoyo, “Essential oil from Cinnamomum cassia bark through hydrodistillation
and advanced microwave assisted hydrodistillation,” Industrial Crops and Products,
vol. 92, pp. 57–66, Dec. 2016.
References

41. 5. N. N. Kasim, S. N. A. S. Ismail, N. D. Masdar, F. Ab Hamid, and W. I. Nawawi,
“Extraction and Potential of Cinnamon Essential Oil towards Repellency and
Insecticidal Activity,” International Journal of Scientific and Research Publications,
vol. 4, no. 7, 2014.
6. M. R. Thakker, J. K. Parikh, and M. A. Desai, “Microwave assisted extraction of
essential oil from the leaves of Palmarosa: Multi-response optimization and
predictive modelling,” Industrial Crops and Products, vol. 86, pp. 311–319, Aug.
2016.
7. N. Jeyaratnam, A. H. Nour, and J. O. Akindoyo, “The potential of Microwave
Assisted Hydrodistillation in extraction of essential oil from cinnamomum cassia
(cinnamon),” 2006.
References

42. Paper publication

43.  Satish Kumar M, “Optimization of Yield for Extraction of an
Essential Oil from Cinnamon using Microwave-Assisted
Extraction”, Journal of Chromatography & Separation
techniques, 2017. ISSN:2157-7064.
Paper publication

44. Questions ?

45. Thank you.