AU2020205227B2 - Method and system for recovering residual plant components - Google Patents

Abstract

A process of extracting bioactive components from plant material comprising the steps of: (a) subjecting plant material to water or steam distillation of essential oils and obtaining post distillation plant material in a distillation chamber; (b) collecting a distillate from the water or steam distillation step (a) and separating the distillate into an essential oil fraction and a hydrosol fraction; (c) directing the hydrosol fraction to the distillation chamber to contact the post distillation plant material under conditions permitting extraction of the one or more bioactive components from the post distillation plant material to obtain a bioactive component enriched hydrosol. ABSTRACT2020205227 14 Jul 2020 FIGURE 1 110 120 122 124 112 130 170 172 180 182 192 194 150 114 154 156 158 157 137 153 20 20 20 52 27 1 4 Ju l 2 02 0Jul 2020 2020205227 14 182 112 192 158 194 122 172 124 114 154

Description

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FIGURE 1

2020205227 14 Jul 2020 METHOD ANDSYSTEM METHOD AND SYSTEMFOR FOR RECOVERING RECOVERING RESIDUAL RESIDUAL PLANT PLANT COMPONENTS COMPONENTS

TECHNICALFIELD TECHNICAL FIELD

[001]The present invention is related to chemical and biological components derived

from plants. In particular, the invention relates to a process for recovering substances

from plant material residue after distillation of essential oils from the material.

BACKGROUND BACKGROUND

[002] Any references to methods, apparatus or documents of the prior art are not to

be taken as constituting any evidence or admission that they formed, or form part of

the common general knowledge.

[003] Plants of a wide variety of species have been used for health promoting and

particular medicinal purposes for many thousands of years. In recent years, research

has revealed that plant-based phenols, flavonoids, isoflavones, terpenes,

glucosinolates and other compounds present in fruits, vegetables and leafy herbs,

among other types of plants, possess antioxidant and anti-carcinogenic properties,

among other health-promoting benefits.

[004] The present invention will be described with particular reference to a

composition derived from Melaleuca alternifolia. However, it will be appreciated that

compositions of the invention may also be sourced from other Melaleuca species and

no limitation is intended thereby. Other suitable sources of compositions of the present

invention include but are not limited to M. linarifolia, M. dissitiflora, M. bracteata, M.

cricifolia and M. quinquinervia.

2020205227 14 Jul 2020

[005] Essential oils are complex mixtures of volatile oils produced by plants and are

responsible for the odor of many plants. The essential oil, once produced, is either

releasedtotothethe released environment environment or stored or stored in oilfor in oil cells cells foruse. later laterEssential use. Essential oils oils stored in stored in

the wood of plants serves to deter microorganisms and insects from attack.

[006] The essential oil obtained from the steam distillation of the stems and leaves of

Melaleucaalternifolia Melaleuca alternifolia is is known knownas as tea tea treetree or Melaleuca or Melaleuca oil. tree oil. Tea Teaoil tree is oil wellis well

characterized and is described at page 1622 of the Thirteenth edition of the Merck

Index 2001, which entry is incorporated herein by reference. Tea tree oil has been

allocated CAS number 68647-73-4, incorporated by reference.

[007] Due to the ever-growing consumer preference for natural products and

remedies, the value of plant derived therapeutic agents has increased steadily.

Moreover, the more traditional value base of certain plant components, e.g., for the

flavor and fragrance industry, has remained robust.

[008] Essential oils constitute one type of valuable plant component. An essential oil

is a concentrated, hydrophobic liquid containing volatile aromatic compounds,

obtained by distillation from various plant parts. Essential oils are used in perfumery,

aromatherapy, cosmetics, incense, for flavouring food and drink, and in medicine. The

medicinal value ofof certain medicinal value certain essential essential oils oils can can be be considerable. considerable.

[009] Essential oils are produced by water or steam distillation. Typically, the plant

material is immersed in water and boiled, or exposed to steam flow. The steam and

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2020205227 14 Jul 2020 oil vapour is condensed and the oil is separated from the water. Customarily, the

residual plant material is discarded once the essential oils have been distilled, on the

assumption that the material would not yield additional components or substances of

appreciable value once it has been subjected to the distillation process. Therefore, it

would be desirable to provide a method for better utilising the residual plant material.

SUMMARYOFOFINVENTION SUMMARY INVENTION

[010] In an aspect, the invention provides a process of extracting bioactive

components from plant material comprising the steps of:

(a) subjecting plant material to water or steam distillation of essential oils

and obtaining post distillation plant material in a distillation chamber;

(b) collecting a distillate from the water or steam distillation step (a) and

separating the distillate into an essential oil fraction and a hydrosol fraction;

(c) directing the hydrosol fraction to the distillation chamber to contact the

post distillation plant material under conditions permitting extraction of the one or more

bioactive components from the post distillation plant material to obtain a bioactive

component enriched hydrosol.

[011] In one embodiment, the plant material is of the Melaleuca species,

Lamiaceae species, Geraniaceae species, Backhousia species,

Leptospermeae species and/or Myrtaceae species.

2020205227 14 Jul 2020

[012] In another aspect, the invention provides a process of extracting bioactive

components from a plant of the Melaleuca species or portion thereof, the process

comprising the steps of:

(a) subjecting plant material of the Melaleuca species to water or steam

distillation of essential oils and obtaining post distillation plant material in a distillation

chamber;

(b) collecting a distillate from the water or steam distillation step (a) and

separating the distillate into an essential oil fraction and a hydrosol fraction;

(c) directing the hydrosol fraction to the distillation chamber to contact the

post distillation plant material under conditions permitting extraction of the one or more

bioactive components from the post distillation plant material to obtain a bioactive

component enriched hydrosol.

[013] In an embodiment, the process of extracting bioactive components in

accordance with further comprises step (d) wherein step (d) comprises collecting the

enriched hydrosol and directing the enriched hydrosol back to the distillation chamber

to contact the post distillation plant material for additional enrichment of the enriched

hydrosol.

[014] In an embodiment, the enriched hydrosol from step (c) or step (d) is sampled

and analysed for concentration of the bioactive components and whereby step (d) is

repeated if the concentration is below a predetermined level and wherein the enriched

2020205227 14 Jul 2020 hydrosol is collected if the concentration is equal to or greater than the predetermined

level. level.

[015] In an embodiment, the process of extracting bioactive components further

comprises an intermediate step of adding a solvent to the hydrosol fraction before

directing the hydrosol fraction to step (c).

[016] In an embodiment, the post-distillation plant material in step (c) and/or (d) is

moist.

[017] In an embodiment, step (c) and/or step (d) further comprises treatment with

steam. In an embodiment, the steam is a low volume of steam.

[018] In an embodiment, step (c) and/or (d) further comprises treatment with

compressed air.

[019] In an embodiment, the solvent is an alcohol. Preferably, the solvent is ethanol.

[020] In an embodiment, step (c) further comprises spraying or sprinkling the hydrosol

on the post distillation plant material to contact the post distillation plant material

thereby extracting the bioactive components into the sprayed or sprinkled hydrosol.

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[021] In an embodiment, the post distillation plant material is positioned on a draining

surface with a plurality of openings to allow the enriched hydrosol to be drained into a

collection chamber positioned under the draining surface.

[022] In an embodiment, conditions for permitting extraction in step (c) further

comprise one or more of the following:

(e) introducing compressed air into the distillation chamber at a pressure in

the range of 1-5 psi and more preferably 2-3 psi; and/or

(f) introducing steam into the distillation chamber.

[023] In an embodiment, step (f) comprises introducing low pressure steam at a

pressure below 50 psi.

[024] In an embodiment, the plant material wherein the plant material comprises one

or more of flowers, seeds, leaves, stems and roots.

[025] In an embodiment, the bioactive components are selected from phenolic

compounds, flavones, isoflavones, glycosides, anthocyanins, proanthocyanidins,

procyanidins, catechins, terpenes, lignins, tannins, glucosinilates, aliphatic and cyclic

organic acids.

[026] In an embodiment, the bioactive component has antioxidant activity.

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[027] In one embodiment, the invention resides in the extracted bioactive

components produced by any of the above aspects.

BRIEF DESCRIPTION OF THE DRAWINGS

[028] Preferred features, embodiments and variations of the invention may be

discerned from the following Detailed Description which provides sufficient information

for those skilled in the art to perform the invention. The Detailed Description is not to

be regarded as limiting the scope of the preceding Summary of the Invention in any

way. The Detailed Description will make reference to a number of drawings as follows:

Figure 1 is a schematic diagram for a system 100 used for extracting bioactive

components from plant material.

DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS

[029] In accordance with various aspects of the present invention, methods are

provided for obtaining substances of interest from plant material that has previously

been subjected to water or steam distillation of essential oils. It has heretofore been

the practice in the industry to discard the residual plant material after distillation of

essential oils, on the assumption that no additional components of appreciable value

could be obtained from such residual material. Contrary to this notion, it has been

discovered in accordance with the present invention that a number of substances can

indeed be retrieved from such plant material, many of which exhibit functional features,

e.g., antioxidant or antimicrobial properties.

2020205227 14 Jul 2020

[030] The methods described herein may be practiced on any plant. Suitable plants

are those with at least one tissue or organ containing a substance or agent that is

extractable by the methods set forth below, and from which essential oils may be

obtained by water or steam distillation.

[031] Any part of the plant from which essential oils are obtained are suitable for

use in the present invention. These include, but are not limited to, flowers, seeds,

bracts and other floral parts, stems, leaves and roots. In certain embodiments, leaves

and stems are utilized. In other embodiments, leaves are utilized.

[032] Plant material for the aforementioned method embodiment was obtained from

Australian native Melaleuca trees, namely Melaleuca alternifolia. However, it will be

appreciated that compositions and methods of the invention may also be sourced from

other Melaleuca species and no limitation is intended thereby. Other suitable sources

of compositions of the present invention include but are not limited to M. linarifolia, M.

dissitiflora, M. bracteata, M. cricifolia and M. quinquinervia.

[033] It will be appreciated that the present invention has been described in relation

to Melaleuca species for ease of description, and the person skilled in the art will

appreciate that the present method can be equally applied to other plant materials. It

will be appreciated that the present invention can be applied to any plant material, in

particular any natural plant material. Non-limiting examples of other plant materials

include Melaleuca species, Lamiaceae species, Geraniaceae species, Backhousia

species, Leptospermeae species and Myrtaceae species. Further non-limiting

examples of plant material include Lavender, Geranium, Rosemary, Lemon Myrtle and

certain Leptospermum and Eucalypts.

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2020205227 14 Jul 2020

[034] Referring to Figure 1. Tea Tree Oil (TTO) was produced by steam distillation of

plant material obtained from the leaves and terminal branches of the Melaleuca tree.

The plant material was subjected to steam distillation in a distillation vessel 110 of

which dimensions are 4m wide, 2m deep and 1.5m high. Steam for carrying out the

distillation was supplied from an external boiler 120 of which capacity is 350 kg water

per hour. One or more steam supply lines 122 were used for supplying steam to the

distillation vessel via steam release ports 124. The steam release ports 124 were

positioned below the plant material to make sure that at least some of the steam

passes through the plant material as it rises through the vessel 110. The steam

flowrate into the distillation chamber 110 may be adjusted automatically by a controller

(not shown) connected to a temperature sensor and a pressure sensor. The typical

operation parameters of the distillation vessel 110 may be 120°C and 20 to 50 psi.

[035] The distillation vessel 110 includes outlets 112 for allowing a mixture of steam

and essential oils extracted from the plant material positioned in the vessel to be

directed to a condenser 130 and a cooler 135 which in turn results in separation of the

distillate into an essential oil fraction and a hydrosol fraction (mainly containing water)

in a separating column 137. The essential oil fraction may be collected in a collection

tank 150 for further processing.

[036] The distillation step described above is an initial step which is followed by a

further treatment step which comprises treatment of the post distillation plant material

170 that has been left behind after the initial distillation step has been completed. The

hydrosol fraction from the separating column 137 is directed via fluid supply lines 182

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2020205227 14 Jul 2020 to a series of spray or sprinkler units 180 to spray the hydrosol on the post distillation

plant material that is placed on a draining surface 172. The inventor has found that

contacting the post distillation plant material 170 with the hydrosol from the separating

column 137 whilst the post distillation plant material is relatively moist is very useful in

allowing bio active components to be extracted out of the post distillation plant

material. A material. lowvolume A low volumeof of steam steam was was also directed also directed intointernal into the the internal volumevolume of the of the

vessel through the steam release ports 124 to maintain the post distillation plant

material 170 in a limp or moist state. The extraction of the bio active components from

the post distillation plant material 170 may be further enhanced by supplying low

pressure steam from the boiler 120 through steam ports 124. Similarly, the extraction

of bio active components may also be enhanced by supplying low volume compressed

air via air inlet ports 192. An air compressor 194 may be used for supplying

compressed air into the internal volume of the distillation chamber 110. Additionally,

in some applications, a solvent in the form of ethanol (at say 20% concentration-non

limiting) may also be introduced into the hydrosol by a solvent introduction port 158

into fluid supply line 182 to further enhance the extraction of bioactive components

into the hydrosol. It is also important to note that the volume of the starting plant

material may be varied.

[037] In one embodiment, the method further includes the step of adding ethanol to

the bioactive component enriched hydrosol. In one embodiment, the ethanol added is

greater than about 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, 15% or 20% by

weight of the bioactive component enriched hydrosol. In one embodiment, the amount

of ethanol added to the bioactive component enriched hydrosol is about 10% by

weight. The additional ethanol is postulated to increase the shelf life of the bioactive

component enriched hydrosol.

2020205227 14 Jul 2020

[038] The typical process of extracting bioactive components from the post distillation

plant material would involve collecting the enriched hydrosol (which would include the

extracted bioactive components) once the sprayed hydrosol has contacted the post

distillation plant material 170 and drained through the draining surface 172 into a

collection container 154 through an outlet port 114. The composition of concentration

of the bioactive components in the enriched hydrosol may be analysed by sampling

the enriched hydrosol via sampling port to check if the concentration or characteristics

are sufficient to meet a pre-determined criteria. If the concentration does not meet the

criteria then the enriched hydrosol may be directed back to fluid supply line 182 and

recycled through another round of enrichment. Therefore, the concentration of the

bioactive components may be progressively increased by way of repeated recycling

of the hydrosol. Once the desired concentration or characteristics have been achieved

the valve controller may be closed to commence collection of the enriched hydrosol.

[039] It is important to appreciate that the process of extracting the bioactive

components is not carried while distillation is occurring. Instead, the bioactive

component extraction process is carried out immediately after or within a reasonable

time period after the distillation process has been completed. Without being bound by

theory, it is hypothesized that the extraction process relies upon post distillation plant

material which may include leaves in a "limp" state which improves extraction of the

bioactive components from the plant material particularly leaves.

[040] It is postulated that the treatment of the post distillation plant material with the

hydrosol is that additional compounds may be recovered that are not extracted by the

distillation process. These extracted compounds can have additional advantageous

2020205227 14 Jul 2020 properties. Furthermore, the enriched hydrosol can be added to products in certain

industries because they are natural ingredients.

[041] The enriched hydrosol sample was tested by Biotest Laboratories from

Underwood, Queensland, Australia on 8th May 2019. Specifically, anti-biotic properties

of the enriched hydrosol sample were tested using challenge microorganisms

including Staphylococcus aureus ATCC 6538, Pseusomonas aeruginosa ATCC 9027,

Escheria coli ATCC 8739, Salmonella typhimurium ATCC 13311 and Candida

albicans ATCC 10231. The test suspension was added to the test sample of the

enriched hydrosol and the mixture was maintained at 250C. At the test contact times,

an aliquot was taken, suitably neutralized, the number of surviving organisms in each

sample was determined and the reduction in viable counts was calculated.

On ew I Initial kloclum RecoeryCounts

CFU per toCUmintes 0wminutes 30 4hou 4 hours 24hours 24 hours

pam gram CFU per Log Percentage CFU per Log Percentage CFU per Log Percentage Reduction Reduction Reduction Reduction Reduction Reduction gram gram gram From Initial From Initial From Initial From Initial From Initial From Initial

count count count count count count

COmid*a~wasATCC10231 3h1 3&1 3O1O 3.2x10 5.2x1A 5.51 5.51 NMR. NMR * &XI . * W Mgt NMR NM NMR NMR* . NMR* NMR . NMR . NMR NMR . Yeast Yeart

Initial Inoculum ChalleeInitinocum Estiate Recovery Counts Based-on Colony Morphology Differentiaton Estimate Recovery Counts Based on Colony Morphology Differentiation

U per Log u 30 minutes hours 24houni

CFU per Log Percentage CFU per Log Percentage Log Percentage CFU per gra Reduction Reduction dm m . Reduction N. RWl Reduction gram RIKM Reduction dWo Reduction

count count count count count count

StMybcD aunsa A Staphylococcus aureus ATCC 6538 S.aureus 2 32 99 5 4AXdW 5.64 d4.'x No No >3.Ox1s N0N15 - 2.32 g95 - Yeast= >3.0x10

PseudomonasaeingkosUoATCC927 NMR UR# # No No No No 3.Ox1W 3.0x10 SAS 5.48 -3.& =3.9x10 reduction N >3.0x10 >o-n reduction reduction - - Yeast= .

>3.0x10

EscherfdIdkco#ATCC8739 Escherichia coll ATCC 8739 E. E.coll

* 2 .5 x10l .59 =97A 1.2xW' 6. ,. =5.7x10 reduction reduction Yeast= >3.0x10

SOmna vjtyphMUwumATCC13311 S. =2.44 No No No No =1.4x10³ 3.9x105 5.59 =4.4x106 >3.0x10 99.6 reduction reduction reduction reduction

>3.0x10

2020205227 14 Jul 2020

Challenge Product TestProduct Control Recovery % lntWpmetlan Orpnlsm Dilution Dilution RecoseryCM SystM Recovery CFU

StaphyorccusaurusATCCGS8 1:10 24.35(30) 23,28(26) 125 RecoV @ Recovery

1 - 1:2D41111ton

Pseudo hasaderugmM ATCC 9027 111 3.4(2) 3272 28 Recoery

& 1:10 30.3(32) 23,7(28) 12

Esdierkidoalf ATOC 8739 2:10 4k 45(4W) 37,38(38) 113 Rcvr LID dilution 1:10 dilution

SalffmwomltphmudumATCC13311 110 19,20(20) 17,21(19) 105 RtoverL 110dilution

CNdidaa/b~consATCC10231 Candida albicans ATCC 10231 110 1:10 Noresultusabletodifferentiatecolonymorphiogy

As evident from the results, the extract performed to a satisfactory level. The results

indicate that a significant reduction was in the count of organism occurred, especially

after 24 hours. Please note that these the extract used in the above tests was alcohol

free, and so it is postulated that the above results are largely if not completely

attributed to the extracted bioactive components.

[042] In compliance with the statute, the invention has been described in language

more or less specific to structural or methodical features. The term "comprises" and

its variations, such as "comprising" and "comprised of' is used throughout in an

inclusive sense and not to the exclusion of any additional features.

[043] It is to be understood that the invention is not limited to specific features shown

or described since the means herein described comprises preferred forms of putting

the invention into effect.

[044] The invention is, therefore, claimed in any of its forms or modifications within

the proper scope of the appended claims appropriately interpreted by those skilled in

the art. the art.

Claims (8)

CLAIMS 11 Dec 2025

1. A process of extracting bioactive components from plant material comprising the steps of:

(a) subjecting plant material to water or steam distillation of essential oils and obtaining post distillation plant material in a distillation chamber; 2020205227

(b) collecting a distillate from the water or steam distillation step (a) and separating the distillate into an essential oil fraction and a hydrosol fraction;

(c) directing the hydrosol fraction to the distillation chamber to contact the post distillation plant material under conditions permitting extraction of the one or more bioactive components from the post distillation plant material to obtain a bioactive component enriched hydrosol,

wherein step (c) is completed without distillation occurring.

2. A process of extracting bioactive components from a plant of the Melaleuca species or portion thereof, the process comprising the steps of:

(a) subjecting plant material of the Melaleuca species to water or steam distillation of essential oils and obtaining post distillation plant material in a distillation chamber;

(b) collecting a distillate from the water or steam distillation step (a) and separating the distillate into an essential oil fraction and a hydrosol fraction;

(c) directing the hydrosol fraction to the distillation chamber to contact the post distillation plant material under conditions permitting extraction of the one or more bioactive components from the post distillation plant material to obtain a bioactive component enriched hydrosol,

wherein step (c) is completed without distillation occurring.

3. The process of claim 1 or claim 2 further comprising step (d) collecting the 11 Dec 2025

enriched hydrosol and directing the enriched hydrosol back to the distillation chamber

to contact the post distillation plant material for additional enrichment of the enriched

hydrosol,

wherein step (d) is completed without distillation occurring. 2020205227

4. The process of any one of the preceding claims, wherein the enriched hydrosol

from step (c) and/or step (d) is sampled and analysed for concentration of the bioactive

components, and whereby step (d) is repeated when the concentration of the bioactive

components is below a predetermined level or the enriched hydrosol is collected if the

concentration of the bioactive components is equal or above the predetermined level.

5. The process of any one of the preceding claims further comprising an

intermediate step of adding a solvent to the hydrosol before directing the hydrosol

fraction to step (c).

6. The process of any one of the preceding claims, wherein the post-distillation

plant material is moist.

7. The process of any one of the preceding claims, wherein step (c) and/or step

(d) further comprises treatment with compressed air.

8. Extracted bioactive components produced by the process of any one of the 11 Dec 2025

preceding claims.

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FIGURE 1