8. extraction by hydro-distillation method hydro-distillation of...

Patel J.B. Chapter 8

K.B.I.P.E.R. Kadi Sarva Vishwavidyalaya, Gandhinagar 172

8. Extraction by Hydro-distillation method

8.1 Hydro-distillation of Cuminum cyminum Linn.

8.1.1 Experimental:

8.1.1.1 Instrumentation:

Pulverizer (Model PP-200, Yagnam pulverizer Private LTD, Navi Mumbai)

Seives (No 30, 40)

Clevenger-type apparatus

GC-MS (6890 GC-5073 MS, Perkin Elmer, USA)

8.1.1.2 Chemicals and Materials:

Cumin seeds were procured from the local market of Unja, Mehsana,

India

8.1.1.3 Experimental procedures:

8.1.1.3.1 Extraction of essential oil from Cuminum cyminum seed powder

Five hundred grams of each aromatic herb were submitted to hydro-distillation with

a Clevenger-type apparatus according to the European Pharmacopoeia and extracted

with 6 L of water for 4.5 h (until no more essential oil was obtained).

The essential oil was collected, dried under anhydrous sodium sulphate and stored

at 0 ◦C until used. The samples were analysed further by GC-MS method.

8.1.1.3.2 Analysis of essential oil by GC-MS

The following parameters were set for the analysis.

• Instrument

– GC-MS (6890 GC-5073 MS, Perkin Elmer, USA)

• Colunm: Fused-silica-capillary column with a stationary phase SBP5TM (60m

× 0.32μm × 1μm film thickness).

• Carrier gas: He

• Flow rate: 0.7 mL/min

• Split: 1:20

• Injection volume: 0.1μL

• Injection temperature: 250 ◦C

• Oven temperature progress from 60 to 130 ◦C at 1◦C/min, from 130 to 200 ◦C

2.8.12.%20Determination%20of%20essential%20oils%20in%20vegetable%20drugs.pdf



at 2◦C/min, from 200 to 250 ◦C at 4 ◦C/min and holding at 250 ◦C for 40 min

• Ionisation mode used was electronic impact at 70 eV. 428-429

8.1.2 Results and discussion

The analysis of the essential oil by GC is reported in figure 8.1.1.1.

Figure 8.1.1.1: GC analysis of the essential oil extracted by hydro-distillation from

seed powder of Cuminum cyminum Linn.



The analysis of the essential oil by GC-MS is reported in previous section in figures

6.1.1.2-6.1.1.7

The results of GC-MS analysis is summarized in following table.

Table 8.1.1.1: The results of the analysis of the GC and GC-MS spectrum of the

different constituents of the essential oil extracted from Cuminum cyminum Linn. by

Hydro-distillation.

Sr No RT Compound % content

HD HD

1 5.925 α-pinene 1.42 19783.13

2 7.099 1-methyl-4-(1-methylethyl)benzene n n

3 7.869 1-methyl-4-(1-methylethyl)-1,4-cyclohexadiene 14 194562.3

4 10.6 D-limonene 0.61 8466.8

5 11.4 Cuminal 16.1 223729.5

6 12.2 2-ethylidene-6-methyl-3,5-heptadienal 28.2 391789.8

7 13.405 Caryophyllene n n

8 16.412 β-terpeneol 0.14 1956.4

9 22.701 Eucalyptol n n

10 23.104 Carinol 9.2 127888.3

11 24.974 3-carene 0.3 4238.8

12 26.533 4-carene 0.4 5483.06

13 26.936 α-propylbenzmethanol 0.9 12390.2

14 40.98 Thujopsene 0.1 1394.01

Total content fraction of determined compounds 71.37 Extraction time 4.5 h % yield 2

Hydro-distillation method was carried out using the apparatus specification given in

European pharmacopoeia with adoption of standard set of procedure. Hence there

was no need of optimizing such procedure. The results of this method were

considered for comparative study of results of novel methods.

The extraction procedure was evaluated on the basis of the total content fraction of

determined compounds, extraction time, percent yield etc. The total fraction

content of determined compounds was found to be 71.37 %. Only those compounds

present in major amount or susceptible to change by extraction procedure were

taken into consideration for assessing the adoptability of such method in comparison

to conventional extraction method. The major constituents enlisted were cuminal, 1-

methyl-4-(1-methylethyl)-1,4-cyclohexadiene,2-ethylidene-6-methyl-3,5-heptadienal



while α-pinene, D-limonene, carinol, 3-carene, 4-carene, α-propylbenzmethanol,

thujopsene were found in minor amount. The yield was 2%. The system was run

upto no more essential oil was liberated.

Hydrolysis of some active constituent is dependent on the amount of water, its

contact time etc. it may be enhanced by temperature also. It can be proved by

classical example of propylbenzmethanol. Direct contact of it with water for longer

period of time enhanced its hydrolysis as compared to the hydrolysis found in

methods like Improved Microwave Assisted Extraction and Supercritical fluid

Extraction.

Cuminal is an aldehyde constituent and is accounted for 16.1 % of the total

constituents.

The extracted oil was having very light yellow colour when it is fresh but after the

storage for one day at refrigerator temperature it became pale yellowish in colour.

The optical rotation and refractive index of the oil was found to be 2.5 and 1.50

respectively. The oil was having typical charred odour.



8.2 Hydro-distillation of Foeniculum vulgare Linn.

8.2.1 Experimental:



Seives (No 30, 40)




Fennel seeds were procured from the local market of Unja, Mehsana,

India

8.2.1.3 Experimental Procedures:

8.2.1.3.1 Extraction of essential oil from Foeniculum vulgare Linn. seed powder



with 6 L of water for 4.5 h (until no more essential oil was obtained).

The essential oil was collected, dried under anhydrous sodium sulphate and stored

at 0 ◦C until used. The samples were analysed further by GC-MS method.



• Instrument




• Carrier gas: He


• Split: 1:20




at 2◦C/min, from 200 to 250 ◦C at 4◦C/min and holding at 250 ◦C for 40 min





8.2.2: Results and discussion:


Figure 8.2.1.1: GC analysis of the essential oil extracted by Hydro-distillation from

seed powder of Foeniculum vulgare Linn.



The analysis of the essential oil by GC-MS is reported in previous section in figures

6.2.1.2-6.2.1.6



different constituents of the essential oil extracted from Foeniculum vulgare Linn. by

Hydro-distillation.


Compound HD HD

1 5.75 α-Limonene 5.4 275222.7

2 7.18 L-fenchone 15 763532.3

3 9.417 Methyl chevicol [(1-methoxy-4-(2-propenyl) benzene) 10 509068.3

4 10.48 Anisic aldehyde (4-methoxy benzaldehyde) 0.5 25451.4

5 11.1 Anethole [(1-methoxy-4-(1-propenyl)-benzene)] 70.2 3572004

6 12.02 palimitic acids n n

7 12.4 γ-terpenene 1.3 65793.7

8 20.76 Myrcene 0.9 45676.6

9 28.55 Caprinone (10-nonadecanone) 0.3 15233.8

10 28.97 Unidetified mass 1.5 76106.2

Total content fraction of determined compounds 105.1 Extraction time 3.5 h % yield 0.4






determined compounds, extraction time, percent yield etc. The total fraction

content of determined compounds was found to be 105.1 %. Only those compounds



to conventional extraction method.

The major constituents enlisted were anethole and fenchone while anisic aldehyde,

terpenene, myrcene, carpinone, α- limonene were found in minor amount. The yield



was 0.4 %. The system was run upto no more essential oil was liberated. The

extracted oil was having light yellow colour.

Presence of anethole in a high percentage makes the oil highly odorous. Methyl

chevicol and anethole are isomeric products. Here the content fraction of methyl

chevicol constitutes about 10 % which is very high as compared to Improved

Microwave Assisted Extraction and Supercritical Fluid Extraction method. It confirms

the effect of temperature in conversion of anethole in methyl chevicol. It may be

further confirmed by comparing the results of GC-MS analysis of extracted oil by

hydro-distillation technique. This method doesn’t able to extract palimitic acid ester.



8.3 Hydro-distillation of Coriandrum sativum Linn.

8.3.1 Experimental:



Seives (No 30, 40)




Coriander seeds were procured from the local market of Unja, Mehsana,

India

8.3.1.3 Experimental Procedures:

8.3.1.3.1 Extraction of essential oil from Coriandrum sativum Linn. seed powder



with 6 L of water for 4.5 h (until no more essential oil was obtained). The essential oil

was collected, dried under anhydrous sodium sulphate and stored at 0 ◦C until used.

The samples were analysed further by GC-MS method.



• Instrument




• Carrier gas: He


• Split: 1:20




at 2◦C/min, from 200 to 250 ◦C at 4◦C/min and holding at 250 ◦C for 40 min





8.3.2: Results and discussion


Figure 8.3.1.1: GC analysis of the essential oil extracted by Hydro-distillation from

seed powder of Coriander sativum Linn.



The GC-MS of compounds has been reported in previous section in figures 6.3.1.2-

6.3.1.10.



different constituents of the essential oil extracted from Coriandrum sativum Linn.

by Hydro-distillation.


HD

1 3.59 β-pinene 1.82

2 4.9 α-pinene 0.05

3 6.63 Terpinen 3.46

4 7.34 Linalool 71.72

5 9.47 Dodecenal 0.18

6 11.19 Undecenal 0.34

7 12.22 geranyl acetate 3.21

8 12.67 Ocemene 0.1

9 13.5 trans β ocemen 0.15

10 16.97 myrtinyl acetate 0.43

12 19.04 myrtinyl acetate (Z) 0.3

16 20.34 oleic acid methyl ester 0.2

18 20.74 octadecenoic acid 21.61

19 23.53 Hexadecenal 0.3

Extraction time 4.0 h

% yield 0.6






determined compounds, extraction time, percent yield etc. Only those compounds



to conventional extraction method.



The major constituents enlisted were Linalool, octadecenoic acid ester while β-

pinene, α-pinene, terpinen, dodecenal, undecenal, geranyl acetate, ocemene, trans

β ocemen, myrtinyl acetate, oleic acid methyl ester, hexadecenal were found in

minor amount. The yield was 0.6 %. The system was run upto no more essential oil

was collected. The extracted oil was having light yellow colour.

8. extraction by hydro-distillation method hydro-distillation of...

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