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A PROCESS FOR EXTRACTION OF ESSENTIAL OIL FROM DRACOCEPHALUM HETEROPHYLLUM BENTH

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Title A PROCESS FOR EXTRACTION OF ESSENTIAL OIL FROM
DRACOCEPHALUM HETEROPHYLLUM BENTH
 
Creator Kaul , V K
Mahmood, U
Ahuja, Paramvir Singh
Lal, Brij
Negi, H R
Singh, Virendra
 
Subject Plant sciences
Natural Product Chemistry
 
Description Complete Specification

The present invention relates to a process for the extraction of essential oil from Dracocephalum heterophyllum benth.
The present invention relates to an essential oil with citronellol and rose oxides in high yield and other perfumery compounds obtained from a cold desert plant source Dracocephalum heterophyllum benth. The present invention also relates to a process for the extraction of essential oil from the plant source. BACKGROUND ART
The generic name Dracocephalum Linn is derived from Greek words Drakon meaning dragon and Kephale meaning head referring to the appearance of the heads of the flowers. The genus Dracocephalum comprises about 50 species distributed in Northern Hemisphere i.e. Southern Europe, North America, North Africa and temperate Asia. Reference may be made to Hooker, J.D. Flora of British India, 1872-97 vol-4, 666, London. Another reference may be made to Bailey, L.H. 1976. Hortus Third (revised edition), MacMillan Co. NY. 398 D. heterophyllum is a native to western Himalaya and Tibet. Reference may be made to Hay, T. 1937. Gard. Chron. 101:203. It is one of the 8 species known so far from Indian subcontinent. D. heterophyllum has been reported from different parts of India including J & K, H.P., Uttaranchal and Sikkim Himalaya between the elevation of 3000-5200m.
Reference may be made to Hooker, J.D. Flora of British India, 1872-97 vol-4, 666, London, another reference may be made to Anon., 1952, vol.-III, PID, New Delhi, yet another reference may be made to Hajra, P.K. and Balodi, Vipin 1995, Plant Wealth of Nanda Devi Biosphere Reserve BSI, Dehra Dun. pp.. 277. This plant has not yet been explained for any commercial utility. But on the basis of recent field studies it has been revealed that the crude extract of the plant is used in treating eye ailments like redness of eye, irritation and conjunctivitis of the native people of Spiti valley, HP. The same use has been reported earlier from Ladakh region of J&K reference may be made to Srivastava, T.N. and Gupta, O.P. 1982 in C.K. Atal and B.N. Kapur (eds.): Cultivation and utilization of medicinal plants PP-519. RRL Jammu.
A literature survey on Dracocephalum shows that the essential oil of many species have been reported. Reference may be made to Ahmedi, L., Mirza, M. (2001).

Volatile constituents of Dracocephallum aucheri Boiss.J. Essent. Oil Res., 13, 202.
The result shows that there are remarkable differences in the major constituents.
On the basis of major chemical constituents of Dracocephalum species, it can be
divided into 5 major chemotypes
1) citral, geraniol type
2) p-mentha-1,8-diene-1 -ol, limonene type
3) 1,8-cineole, limonene, p-cymene type
4) Sabinene, germacene type and
5) Pinocamphone, b-pinene type.
Reference may be made to Misra, L.N., Shawl, A.S. Raina, and V.K. (1988) Volatile
constituents of Dracocephalum nutans. Planta Med. 53, 165.
Keeping in view the significant chemical diversities in essential oil this genus, a detail
study of the essential oil of D.heterophyllum is undertaken. However, some of the
chemical constituents of the essential oils of this plant have been reported recently.
Reference may be made to Lu-Man, Tian-Xuan, Lu-M, Tian-X, (1999), Analysis of
essential oil of D. heterophyllum 34, 925.
Recently, the plant material (whole plant) of D. heterophyllum has been collected
from nature i.e. Shagtal-Gete (4400-4500m) and Kibber (4100-4200m) of Lahul-Spiti
region in Himachal Pradesh in the month of August 2001.
The study has been carried out to analyze its essential oil constituents and it is
revealed that D. heterophyllum has an interesting chemo-rype containing highest
content of citronellol and rose oxides. These yields are substantially higher than any
other reported species of Dracocephalum and is designated 6th type of chemo-type
and named it as citronellol, rose oxide type.
Acclimatization process of this plant in ex-situ conditions i.e. in the experimental farm
(under controlled condition) of the Institute at Palampur (1300m) has also been
carried out to perform comparative studies of the essential oil this plant.
In order to collect ethnobotanical, ecological and floristic field data from higher
altitudes of western Himalaya, a field survey was conducted in Spiti valley of Lahul-
Spiti district of Himachal Pradesh, India in the month of August 2001.
While conducting field surveys in the said area, some patches of D. heterophyllum
Benth. were located near by Gete (4400-4500m) and Kibber (4100-4200m) Villages
in Spiti valley. Population sampling of the same was carried out and simultaneously
plant material (whole plant) was collected for chemical examination. The voucher
The authenticity of the species was confirmed by way of matching with the specimens
documented in the herbarium of Northern Circle, Botanical Survey of India (BSD) Dehra
Dun.
OBJECTS OF THE PRESENT INVENTION
The main object of present invention is to discover a cold desert plant as a new source of
essential oil.
Another object of present invention is to identify/select D. heterophyllum as a new source
of perfumery compounds of commercial significance.
Still another object of present invention is the domestication and cultivation of this plant
for essential oil production.
Further object of present invention is to conduct the comparative studies of the essential
oils of both wild and cultivated populations of D. heterophyllum so as to select the elite
clones.
Still another object of present invention is to discover a high yielding natural source of
citronellol and rose oxides.
Yet another object of present invention is to harness the potential of this natural plant
resource for the economic benefits of the native people living in high mountains.
SUMMARY OF THE INVENTION
The present invention provides an essential oil with citronellol and rose oxides in high
yield and other perfumery compounds obtained from a cold desert plant source
Dracocephalum heterophyllum benth. The present invention also relates to a process for
the extraction of essential oil from the plant source.
DETAILED DESCRIPTION OF THE INVENTION
Accordingly, the present invention provides process for the extraction of essential oil from Dracocephalum heterophyllum benth, wherein the said process comprising the steps of:
[a] charging the said plant material with water in a preferable ratio of 1:2 in a round bottom flask attached to Clevenger type apparatus;
[b] heating the plant material as obtained from step (a) to boiling temperature;
[c] condensing the vapor to separate out the volatile oil from the upper layer of distillate to obtain the desired essential oil composition followed by measuring the quantity of the constituents thereof.

An embodiment of the present invention, wherein the constituents of said essential oil are
identified by Gas Chromatography (GC) and Gas Chromatography Mass Spectra (GCMS).
Another embodiment of the present invention, wherein said oil content is a new
commercial source for citronellol.
Yet another embodiment of the present invention, wherein said oil content is a new
commercial source for cis and trans rose oxides.
Still another embodiment of the present invention, wherein said oil content is a new
commercial source for citronellyl acetate, geranyl acetate and citronellyl iso-butyrate.
Yet another embodiment of the present invention, wherein the yields of citronellol and rose
oxide thus obtained are substantially higher than from any other Dracocephalum species.
Still another embodiment of the present invention, wherein the chemo-type containing
highest content of citronellol and rose oxides is designated as 6th type of chemo-type and
named as citronellol, rose oxide type.
Further embodiment of the present invention, wherein the essential oil yield from D.
heterophyllum is about 0.45% on fresh wt. basis.
The present invention also provides a process for the extraction of essential from a new
plant source, Dracocephalum heterophyllum Benth, said process comprising the steps of:
(a) charging plant material with water in a round bottom flask attached to Clevenger type apparatus;
(b) heating the plant material to a boiling temperature;
(c) condensing the vapor to separate the volatile oil from the upper layer of distillate to obtain the essential oil;
An embodiment of the present invention, a process wherein the essential oil yield from D. heterophyllum is about 0.45% on fresh wt. basis.
Yet another embodiment of the present invention, a process wherein the plant material is selected from the whole plant.

material is selected from the whole plant.
Still another embodiment of the present invention, a process wherein the plant
material is used obtained both from high altitude natural plants and from low altitude
cultivated plants.
Further embodiment of the present invention, wherein D. heterophyllum is cultivated
in the experimental farm (under controlled condition) of the Institute at Palampur
(13300m) and essential oil is distilled on Clevenger apparatus by hydrodistillation
yield 0.4% on fresh wt. basis.
Yet another embodiment of present invention, wherein the GCMS of the essential oils
was carried out on Shimadzu instrument using CP Sil 8CB, non-polar column (5%
phenyl polysiloxane), column length 30 mts (i.d. 0.25 mm) carrier gas helium,
temperature programmed from 100°C-250°at the rate of 6°C/min.
EXAMPLE
Method of extraction of essential oil
1kg of fresh plant material was charged along with water in 1:2 ratio in a 5 litre round
bottom flash. This flash is attached to a Clevenger type apparatus and the whole
system is put on heating mental and heated. After few minutes the material inside start
boiling. The vapour so formed is condensed through condenser in Clevenger type
apparatus. The condensed distillate get collected in a measuring tube, this process is
continued for 3h and the volatile oil is separated from upper layer from the distillate
because of its density difference, as oil is lighter than water and the quantity of oil is
measured.
ADVANTAGES
The present invention will open new vistas in R&D leading to harness the potential of
D. heterophyllum at commercial level by identifying an alternate promising source of
two isomers cis and trans- rose oxides, the highly significant perfumery compounds in
addition to rose and geranium oils.
This plant contains highest percentage of citronellol among the known sources of
Dracocephalum species and can be utilized as an alternate source of this compound.


We claim;
1. A process for the extraction of essential oil from Dracocephalum heterophyllum
benth, wherein the said process comprising the steps of:
[a] charging the said plant material with water in a preferable ratio of 1:2 in a round bottom flask attached to Clevenger type apparatus;
[b] heating the plant material as obtained from step (a) to boiling temperature;
[c] condensing the vapor to separate out the volatile oil from the upper layer of distillate to obtain the desired essential oil composition followed by measuring the quantity of the constituents thereof.
2. A process as claimed in claim 1, wherein the constituents of the essential oil are
identified by Gas Chromatography and Gas Chromatography Mass Spectra.
3. A process as claimed in claim 1, wherein the yield of the essential oil obtained is
at least up to 0.45% on fresh weight basis.
4. A process as claimed in claim 1, wherein the plant material used is whole plant and
obtained from both high altitude natural plant and low altitude new chemotype
named as 6th type of citronellol-rose oxide type chemotype.
5. A process as claimed in claim 1, wherein the mixture of the isolated essential oil comprises in wt%:
[a] cis-rose oxide (0.6-1.6 %),
[b] trans-rose oxide (0.3-0.5%),
[c] citronellal (2.5-6.7%),
[d] citronellol (54.3-74.9%),
[e] geranial (1.5-2.4%),
[fj citronellyl acetate (6.7-21.6%), [g] neryl acetate (0.4-0.7%),

[h] geranyl acetate (1.3-11.7%),
[i] spathulenol (0.2-1.5%),
[j] citronellyl-isobutyrate (0.3-0.8%),
[k] citronellol formate (0-0.2%),
[1] alpha-bourbonene (0-0.4%),
[m] benzaldehyde (0-0.2%),
[n] 6-methylheptanone (0-0.2%),
[o] neral (0-1.2%),
[p] alpha-pinene (0-0.5%),
[q] beta-pinene (0-0.2%),
[r] linalool (0-0.8%),
[s] beta-farnesene (0-0.1%) and
[t] delta-elemene (0-0.5%).
6. A process for the extraction of essential oil from Dracocephalum heterophyllum benth substantially as herein described in the specification.
 
Date 2008-09-29
 
Type Patent
NonPeerReviewed
 
Format application/pdf
 
Identifier http://ihbt.csircentral.net/1030/1/India.pdf
csir, ihbt (2008) A PROCESS FOR EXTRACTION OF ESSENTIAL OIL FROM DRACOCEPHALUM HETEROPHYLLUM BENTH. 01447/DELNP/2003 (223451).
 
Relation http://ihbt.csircentral.net/1030/