U.S. patent application number 09/741551 was filed with the patent office on 2002-10-10 for heated alcohol extraction of herbs.
This patent application is currently assigned to ALTICOR INC.. Invention is credited to Brovelli, Ernesto A., Menon, Gopi R., Vergel de Dios, Luis I..
Application Number | 20020146473 09/741551 |
Document ID | / |
Family ID | 24981172 |
Filed Date | 2002-10-10 |
United States Patent
Application |
20020146473 |
Kind Code |
A1 |
Menon, Gopi R. ; et
al. |
October 10, 2002 |
HEATED ALCOHOL EXTRACTION OF HERBS
Abstract
The present invention relates to methods for the extraction of
herbs and plant materials. More particularly, the present invention
relates to extraction methods for Echinacea. The extraction methods
of the present invention provide a higher soluble solids content
and a higher level of desired marker compounds, such as
alkylamides, than conventional extraction procedures. Thus, the
extraction methods of the present invention result in a greater
yield at a lower cost from a given amount of starting material.
Inventors: |
Menon, Gopi R.; (Riverside,
CA) ; Brovelli, Ernesto A.; (Corona, CA) ;
Vergel de Dios, Luis I.; (Walnut, CA) |
Correspondence
Address: |
WARNER NORCROSS & JUDD LLP
900 FIFTH THIRD CENTER
111 LYON STREET, N.W.
GRAND RAPIDS
MI
49503-2487
US
|
Assignee: |
ALTICOR INC.
|
Family ID: |
24981172 |
Appl. No.: |
09/741551 |
Filed: |
December 19, 2000 |
Current U.S.
Class: |
424/737 |
Current CPC
Class: |
A61P 17/02 20180101;
A61K 36/28 20130101; A61P 37/04 20180101; A61P 31/00 20180101; A61P
37/02 20180101; A61P 29/00 20180101 |
Class at
Publication: |
424/737 |
International
Class: |
A61K 035/78 |
Claims
What is claimed:
1. A method of producing a plant extract comprising: a) providing
plant material; b) contacting the plant material with an alcohol
solution to form a mixture, the alcohol solution comprising about
70% alcohol and about 30% water by weight, and being used in an
amount sufficient to yield a ratio of about 1:10 by weight of plant
material to alcohol; c) heating the mixture to at least about
60.degree. C.; d) maintaining the temperature of the mixture at for
at least about 2 hours, thereby yielding a liquid extract and
non-soluble solids.
2. The method of claim 1 further comprising: a) separating the
non-soluble solids from the liquid extract; b) distilling at least
a portion of the alcohol off of the liquid extract by raising the
temperature of the liquid extract to a temperature above the
boiling point of the alcohol.
3. The method of claim 1 further comprising agitating the mixture
in step d.
4. The method of claim 1 wherein the alcohol is ethanol.
5. The method of claim 1 wherein the plant material is
Echinacea.
6. The method of claim 2 further comprising filtering the liquid
extract.
7. The method of claim 6 wherein the filter has a mesh of about 200
mesh or greater.
8. A plant extract having a high level of desired marker compounds,
produced by a high temperature extraction process, comprising the
following steps: a) providing plant material; b) contacting the
plant material with an alcohol solution to form a mixture, the
alcohol solution comprising about 70% alcohol and about 30% water
by weight, and being used in an amount sufficient to yield a ratio
of about 1:10 by weight of plant material to alcohol; c) heating
the mixture to about 60.degree. C.; d) maintaining the temperature
of the mixture at about 60.degree. C. for at least about 2 hours,
thereby yielding a liquid extract and non-soluble solids.
9. A method of producing a plant extract comprising: a) providing
plant material; b) contacting the plant material with an alcohol
solution to form a mixture, the alcohol solution being used in an
amount sufficient to yield a predetermined ratio of plant material
to alcohol; c) heating the mixture to between about 50.degree. C.
and about 65.degree. C.; d) maintaining the temperature of the
mixture for between about 90 and about 120 minutes, thereby
yielding a liquid extract and non-soluble solids.
10. The method of claim 7 wherein the alcohol solution is between
about 50% to about 90% ethanol.
11. The method of claim 7 wherein the alcohol solution is between
about 60% to about 80% ethanol.
12. The method of claim 7 wherein the alcohol solution is between
about 65% to about 75% ethanol.
13. The method of claim 7 wherein the alcohol solution is 70%
ethanol.
14. The method of claim 7 wherein the ratio of plant material to
alcohol is between about 1:7 and about 1:10 by weight.
15. The method of claim 7 wherein the ratio of plant material to
alcohol is about 1:10 by weight.
16. The method of claim 1 further comprising: a) separating the
non-soluble solids from the liquid extract; b) distilling at least
a portion of the alcohol off of the non-soluble solids and
recovering the distilled alcohol.
17. A method of producing a tablet that contains a plant extract
comprising: a) providing plant material; b) contacting the plant
material with an alcohol solution to form a mixture, the alcohol
solution comprising about 70% alcohol and about 30% water by
weight, and being used in an amount sufficient to yield a ratio of
about 1:10 by weight of plant material to alcohol; c) heating the
mixture to between about 50.degree. C. and about 65.degree. C.; d)
maintaining the temperature of the mixture for between about 90 and
about 120 minutes, thereby yielding a liquid extract and
non-soluble solids. e) separating the non-soluble solids from the
liquid extract; f) drying the liquid extract to form a powder
extract; and g) directly compressing the powder extract with other
excipients to form a tablet.
Description
BACKGROUND OF THE INVENTION
[0001] The present invention relates to novel methods for the
extraction of herbs and plant materials. More particularly, the
present invention relates to extraction methods for Echinacea. The
extraction methods of the present invention provide a higher
soluble solids content and a higher level of desired marker
compounds, such as alkylamides, than conventional extraction
procedures. Thus, the extraction methods of the present invention
result in a greater yield at a lower cost from a given amount of
starting material.
[0002] Typical processes for the extraction of nutrients from herbs
use water or alcohol. In traditional processes, however, ambient
temperature water or alcohol is generally used for the extraction.
Typical processes involve taking the herb, milling it, and
extracting the herb with alcohol and water at some strength of
alcohol, generally 70% to 90%, for a few hours to extract soluble
solids and nutrients.
[0003] Echinacea contains numerous active phytochemicals that have
immunomodulatory and other beneficial activities. There is a long
tradition of the use of Echinacea preparations in the adjuvant
therapy of inflammations, skin damage, and, more typically,
infections. The Echinacea plant is a popular herbal
immunostimulant. The ability of Echinacea to stimulate the immune
system in a nonspecific manner is exemplified in the enhancement of
phagocytosis seen in cells treated with Echinacea (see, Sun et al.,
The American coneflower: a prophylactic role involving nonspecific
immunity, J. Altern. Complement Med., 5(5): 437-446 (1999)).
Echinacea's immunomodulatory activity has been attributed to
various actives, including alkylamides, phenolics, polysaccharides,
alkaloids, glycoproteins, and flavonoids (see, Bauer, R. and
Wagner, H., Echinacea species as potential immunostimulatory drugs,
in Economic and Medicinal Plant Research, Ch. 8, p.253, Wagner, H.
and Farnsworth, N. R. (Editors), Academic Press Limited, New York,
N.Y., (1991)).
[0004] It is, therefore, desirable to develop more efficient and
cost-effective methods of extracting nutrients from herbs such as
Echinacea.
SUMMARY
[0005] The present invention relates to novel methods for the
extraction of herbs and plant materials. The extraction methods of
the present invention result in greater yields at lower cost than
conventional extraction processes.
[0006] In one aspect, the present invention relates to extraction
methods that result in higher yields of soluble solids than
conventional extraction processes.
[0007] In another aspect, the present invention relates to
extraction methods that result in higher levels of marker
compounds, such as alkylamides, than conventional extraction
processes.
[0008] In another aspect, the present invention relates to
extraction methods that yield material with better tableting
characteristics than conventional extraction processes.
[0009] In another aspect, the present invention relates to
extraction methods that are lower in cost than conventional
extraction processes. The methods of the present invention result
in better quality yields and higher yields from a given amount of
starting material, thereby decreasing the cost of the final
product.
BRIEF DESCRIPTION OF SEVERAL VIEWS OF THE DRAWINGS
[0010] FIG. 1 is a flow chart illustrating an herb extraction
process according to the present invention.
[0011] FIG. 2 is a flow chart illustrating a preferred embodiment
of an herb extraction process according to the present
invention.
[0012] FIG. 3 is a flow chart illustrating one preferred embodiment
of an Echinacea root extraction processing according to the present
invention.
[0013] FIG. 4 is a graph illustrating the percent of soluble solids
from heated and unheated Echinacea purpurea extractions using a
10:1 alcohol to root ratio.
[0014] FIG. 5 is a graph illustrating the percent of soluble solids
from heated and unheated Echinacea angustifolia extractions using a
10:1 alcohol to root ratio.
[0015] FIG. 6 is a graph illustrating moisture uptake of Echinacea
purpurea extractions using a 10:1 alcohol to root ratio.
[0016] FIG. 7 is a graph illustrating moisture uptake of Echinacea
angustifolia extractions using a 10:1 alcohol to root ratio.
DETAILED DESCRIPTION OF THE INVENTION
[0017] In accordance with the present invention, novel methods for
the extraction of herbs and plant materials are provided. The
extraction methods of the present invention provide greater yields
at lower costs than conventional extraction processes. The novel
extraction methods of the present invention yield a product with
higher yields of soluble solids, higher levels of marker compounds,
such as alkylamides, and better tableting characteristics than
conventional extraction processes.
[0018] Although the experiments described herein use Echinacea
angustifolia and Echinacea purpurea, the contemplated scope of
present invention is not limited to these two species, or to
Echinacea species in general, but includes all species of herbs or
plant materials. Presently preferred, however, are Echinacea
angustifolia and Echinacea purpurea which are used in the
experiments described herein.
[0019] Experiments were carried out to determine optimal extraction
conditions to yield maximum soluble solids. Maximizing soluble
solids is important to keep the cost of extraction low while
maintaining a high yield of dry extract.
[0020] The extraction process is generally illustrated in FIG. 1.
The extraction process can be used for any type of herb or plant
material. Before starting the batch, all equipment used for
processing is cleaned and sanitized. A sample of starting material
(the dried herb root) is collected for analysis. The raw starting
material is weighed and added to the extraction tank (12). An
alcohol solution is fed into the extraction tank (12). The
extraction tank (12) is heated and the contents of the tank are
preferably agitated during the extraction. The extraction is
carried out for about two hours, maintaining temperature and
agitation throughout. The percentage of soluble solids present is
monitored during the extraction, for example, by measuring the
refractive index.
[0021] After the extraction, the contents of the extraction tank
are preferably cooled to ambient temperature by circulating cool
water through the jacket of the extraction tank. The non-soluble
solids are then separated from the liquid extract with a separation
device (14). Separation can be carried out, for example, using a
filtration device, a centrifuge, a screw press, or any other
separation device. At this point, a sample of liquid extract may be
collected for analysis of desired marker compounds.
[0022] The liquid extract is loaded into an evaporator (16), and
the temperature is raised in order to distill off the alcohol.
Distillation is complete when the alcohol stops boiling off. This
can be confirmed by measuring the percent of soluble solids in the
concentrate. The target for soluble solids is about 9-11% after
distillation is complete.
[0023] The liquid extract is then concentrated by evaporation to a
target level of soluble solids and transferred to covered
containers. The target level of soluble solids depends on the end
use of the product. The liquid extract is generally concentrated to
a target level from about 2 to 3% soluble solids to about 20 to 45%
soluble solids in the concentrate for applications where one spay
dries, freeze dries, tray dries, or vacuum dries the concentrate to
produce a powdered extract. The powdered extract can then be used
as granules or used "as is" to make tablets, two-piece hard shell
capsules, or other forms. The liquid extract can also be
concentrated from about 2 to 3% soluble solids to about 20 to 30%
soluble solids and alcohol (grain or organic) can be added to make
a spray-type product or a dropper-type product.
[0024] Using Echinacea, a series of experiments were conducted to
determine the optimal conditions for the extraction process.
Alcohol concentrations between 50% and 90% alcohol were tested. An
alcohol concentration of about 70% was found to be optimal. Lower
alcohol concentrations yield a lower levels of soluble solids.
Higher alcohol concentrations of about 85% to 90% can yield a
higher level of alkylamides, but the yield of other important
phytochemicals, such as polysaccharides are reduced. Additionally,
using the higher alcohol concentrations greatly increases the cost
of the extraction process and may therefore be cost
prohibitive.
[0025] Various extraction temperatures ranging from ambient
temperature (approximately 18.degree. C. to 24.degree. C.) to about
70.degree. C. were tested. The yield of soluble solids from the
extraction generally increases with increasing extraction
temperature. As the extraction temperature reaches about 65.degree.
C. to 70.degree. C., nearing the boiling point of alcohol, there
are increased emissions from the heated alcohol. The extraction
temperature of about 60.degree. C. was found to be optimal.
[0026] The extraction time was also tested. As seen in Table 1 and
Table 2, the yield of soluble solids generally peaks at about
105-120 minutes of extraction. Many experiments were carried out
with longer extraction times, but extraction times of up to about
6.3 hours have a shown similar mass of soluble solids and similar
alkylamides yields as the 2-hour extraction. Longer extraction
times yield diminishing returns and significantly increase the cost
of the extraction, as found in experiments conducted with
extraction times up to about six hours. Therefore, an extraction
time of about 2 hours is considered optimal.
[0027] A preferred embodiment of the extraction process for
Echinacea is illustrated in FIG. 2 and FIG. 3. A manufacturing
batch size would contain, for example, 400 Kg Echinacea and 4000 Kg
ethanol (1260 gallons). Before starting the batch, all equipment
used for processing is cleaned and sanitized. One (1) Kg of
starting material is collected for analysis. The starting material
is stored in an herb storage tank (24). The raw starting material
is weighed and added to the extraction tank (26). An ethanol/water
mixture is made of about 70% ethanol and 30% water in a quantity
sufficient to give a 1:10 ratio (weight: weight) of raw herb
material to solvent. The ethanol/water mixture is stored in an
alcohol storage tank (22). The alcohol is then fed into the
extraction tank (26). The extraction tank (26) is heated to
60.degree. C./140.degree. F., and the contents of the extraction
tank (26) are agitated during the extraction. The extraction is
carried out for about two hours after reaching 60.degree.
C./140.degree. F., maintaining temperature and agitation
throughout. The percentage of soluble solids present is monitored
during the extraction. Soluble solids can be measured, for example,
by measuring the refractive index of the extract with a
refractometer or through a loss on drying (LOD) technique.
[0028] After the extraction is complete, the contents of the tank
are preferably cooled to ambient temperature by circulating cool
water in the jacket of the extraction vessel. The slurry from the
tank is then pumped out to separate the non-soluble solids from the
liquid extract using a separation device (14). Separation can be
carried out, for example, using a filtration device, a centrifuge,
a screw press, or any other separation device. In one preferred
embodiment, a shaker screen (28) and a screw press (30) are used to
separate the liquid extract from the solids (referred to as cake or
marc). At this point, a 100 ml sample of liquid extract may be
collected for analysis of alkylamides.
[0029] The liquid extract from both the shaker screen (28) and the
screw press (30) are transferred to a storage tank (38). From the
storage tank (38), the liquid extract is loaded into an evaporator
(40), and the temperature is brought to about 77.degree.
C.(170.degree. F.), to distill off the alcohol. Distillation is
complete when the alcohol stops boiling off. This can be confirmed
by measuring the percent of soluble solids in the concentrate. The
target for soluble solids is about 9-11% after distillation is
complete. A 100 ml sample of the liquid concentrate is collected
for analysis of alkylamides.
[0030] The liquid extract is then concentrated through evaporation.
The evaporation is carried out in an evaporator (40) to a target of
about 25%.+-.2% soluble solids. The level of soluble solids is
monitored using a refractometer every 30 minutes until the target
is achieved. Depending on the desired end product, the liquid
extract is then optionally filtered through a filter (42) to remove
remaining insoluble solids. For example, if the end product is a
liquid (for dropper or spray-type product), it is desirable to
filter off any insoluble solids. For a liquid product, the extract
is preferably filtered through a filter with a minimum of at least
about a 200 mesh. This removes particulate matter that could
otherwise interfere with the delivery of the liquid product by, for
example, clogging a spray bottle. Alternatively, if the end product
is a solid powder, it is not necessary to remove remaining
insoluble solids.
[0031] At this point, the concentrated liquid extract is frozen and
stored if it is not to be further processed with 24 hours. As
processing continues, the concentrated liquid extract is then
pasteurized in a pasteurizer (46) at 240.degree. F. for two minutes
to kill any bacteria that may be present in the extract. From the
pasteurizer (46), the extract is further processed for a liquid end
product or a powder end product. For a liquid end product, the
extract is transferred to a liquid product container (48) and
organic alcohol is added to produce a liquid Echinacea product.
[0032] Alternatively, if a dry product is desired, the extract is
transferred to a spray dryer (50). Maltodextrin is added in an
amount equal to 50% of the mass of the soluble solids present in
the liquid concentrate, and the product is spray dried. The
spray-dried powder can then be blended with other ingredients
and/or formed into tablets for the final product.
[0033] In one preferred embodiment, the extraction process includes
a solvent recovery system. After the initial extraction, the
non-soluble solids are separated from the liquid extract using a
separation device (14, FIG. 1) (28 and 30, FIG. 2). After
separation, the non-soluble solids are transferred to a solvent
recovery unit (32) in which the alcohol solvent is dried off of the
non-soluble solids. The non-soluble solids are separated and
discharged appropriately. The recovered solvent is stored in a
reclaimed alcohol tank (36). The recovered alcohol can then be
reused in subsequent extractions. The solvent recovery system
increases the efficiency and reduces the cost of extraction. It is
possible to recover up to 95% of the alcohol used in the
extraction. Additionally, by removing the alcohol from the dried
cake or marc (the non-soluble solids), the solids can be more
easily disposed of.
[0034] In another series of experiments, four alcohol extraction
processes were carried out using the roots of each of two Echinacea
species: Echinacea purpurea and Echinacea angustifolia. The raw
material was Trout Lake Farm tea-cut in all cases. The two
variables for each root extraction process were (1) the alcohol to
root ratio (by weight), and (2) the temperature at which the
extraction was carried out. The two alcohol to root ratios used
were (a) 10:1 and (b) 7:1. The two temperatures used were (a)
unheated, or ambient temperature (approximately 65.degree. F. to
75.degree. F., or 18.degree. C. to 24.degree. C.) and (b) heated,
or approximately 60.degree. C./140.degree. F. For each extraction,
the process included extraction, concentration, and spray
drying.
[0035] Unexpected and surprising results were found with the
extraction using heated alcohol at a 10:1 alcohol to root ratio in
the case of both Echinacea purpurea and Echinacea angustifolia
roots. The heated extractions using a 10:1 alcohol to root ratio
generally produced 40% to 50% more soluble solids, concentrated
well, and spray dried (with M510-Maltodextrin) at a higher
efficiency to produce a better spray dried powder (one that was
non-sticking and had lower moisture uptake) compared to the
unheated extractions.
[0036] Table 1 and FIG. 4 show the percent of soluble solids
present in both heated and unheated Echinacea purpurea extractions
using a 10:1 alcohol to root ratio. Table 2 and FIG. 5 show the
percent of soluble solids present in both heated and unheated
Echinacea angustifolia extractions using a 10:1 alcohol to root
ratio. The heated extractions yield higher levels of soluble solids
throughout the course of the extraction.
1TABLE 1 Percent soluble solids from heated and unheated Echinacea
purpurea extractions using a 10:1 alcohol to root ratio 15 min. 30
min. 60 min. 90 min. 105 min. 120 min. 150 min. Unheated 0.37%
0.73% 0.89% 1.10% 1.45% 1.29% 1.28% Heated 0.70% 0.85% 1.35% 1.90%
1.86% 1.86% 1.75%
[0037]
2TABLE 2 Percent soluble solids from heated and unheated Echinacea
angustifolia extractions using a 10:1 alcohol to root ratio 15 min.
30 min. 60 min. 90 min. 105 min. 120 min. 150 min. Unheated 0.80%
0.95% 1.12% 1.20% 1.78% 1.70% 1.65% Heated 1.14% 2.35% 2.60% 2.40%
2.49% 2.34% 2.30%
[0038] Powder characteristics were compared for each of the four
extract samples (Echinacea purpurea, heated and unheated, and
Echinacea angustifolia , heated and unheated). All of the samples
have "no flow." No flow is a measure of the stickiness or
flowability of a material, and can be measured by the rate at which
a material flows through a cone or funnel. For tableting, no flow
is a characteristic that is not preferred. The samples with the
best powder characteristics, however, were the powders made with
the heated alcohol extraction process.
[0039] Table 3 shows the results for moisture uptake for
spray-dried extracts of Echinacea purpurea and Echinacea
angustifolia prepared by both the heated and unheated extraction
methods. FIG. 6 illustrates the results for moisture uptake for
spray dried extracts of Echinacea purpurea prepared using a 10:1
alcohol to root ratio. FIG. 7 illustrates the results for moisture
uptake for spray dried extracts of Echinacea angustifolia prepared
using a 10:1 alcohol to root ratio.
3TABLE 3 Moisture Uptake of Echinacea purpurea and Echinacea
angustifolia extractions. Time in Minutes 0 60 90 150 270 390 min.
min. min. min. min. min. E. purpurea 0 3.29% 5.65% 7.01% 8.44%
9.28% 1:10, unheated E. purpurea 0 2.6% 5.04% 6.15% 8.2% 9.14%
1:10, heated E. angustifolia 0 3.35% 5.29% 6.62% 8.62% 9.73% 1:10,
unheated E. angustifolia 0 3.11% 4.8% 6.2% 8.01% 9.02% 1:10, heated
E. purpurea 0 2.73% 5.68% 6.44% 8.55% 9.55% 1:7, unheated E.
purpurea 0 4.06% 5.1% 5.26% 6.15% 6.7% 1:7, heated E. angustifolia
0 3.3% 5.47% 6.34% 7.61% 8.28% 1:7, unheated E. angustifolia 0
1.87% 3.7% 5.15% 7.32% 8.6% 1:7, heated
[0040] Moisture uptake is measured as the percent increase in
weight of the spray-dried powder over time. As illustrated in Table
3, the spray-dried powder from the heated extractions absorbs less
moisture than that of the unheated extractions. For example,
spray-dried powder extract of Echinacea purpurea root, prepared
using a 10:1 alcohol to root ratio, showed moisture uptake of 3.29
percent after 60 minutes from the unheated extraction, but only 2.6
percent after 60 minutes from the heated extraction. The moisture
uptake data at 60 minutes is of particular interest because that is
the approximate length of time during which the powder extract is
exposed to air before tableting. The less moisture absorbed by the
extract, the better the tableting characteristics of the
powder.
[0041] In contrast, material extracted with unheated alcohol did
not have any flow, was lumpy, and had a high moisture uptake. This
material could not be tableted. (See Table 4, Column L). Material
extracted with unheated alcohol had a very high ratio of raw
material to dry extract. In other words, with the unheated alcohol
extraction, much more starting material was required to yield a
given amount of dry extract product (See Table 4, Column K).
[0042] Alkylamides, which are used as a marker compounds, are
generally present in commercially available Echinacea at a level of
about 0.5% alkylamides for Echinacea angustifolia , and about 0.1%
for Echinacea purpurea . Using the extraction methods of the
present invention, Echinacea angustifolia extracts have a level of
alkylamides between 0.5% to 2.4%, with an average of 0.95%, and
Echinacea purpurea extracts have a level of alkylamides between
0.136% to 0.534%, with an average of 0.25%. The extraction methods
of the present invention, therefore yield a higher level of desired
marker compounds.
[0043] The following examples describe extractions of Echinacea
purpurea and Echinacea angustifolia according to the methods of the
present invention. The results from these examples is summarized in
Table 4.
EXAMPLE 1
[0044] Echinacea purpurea root
[0045] Alcohol to root ratio: 10:1
[0046] Temperature: unheated (ambient)
[0047] (Table 4, line 1).
[0048] Batches of 50 kg of root (tea cut) were used. The alcohol to
root ratio was 10:1, and the concentration of the alcohol used was
70% (70% EtOH and 30% water). The alcohol was unheated. The 50 kgs
of root were introduced into the tank through the manhole. Once the
raw material was batched into the tank with 70% EtOH/30% H.sub.2O,
a 2-hour extraction was started. Samples were taken at 15-minute
intervals to check soluble solids level.
[0049] Mass Balance: 50 kgs+391 kgs ethanol (200 proof)+150 kgs
H.sub.2O=493.5 kgs of liquid extract+97.5 kgs Cake (1.29% solids)
(60% to 65% moisture)
[0050] The solids were separated from the liquid in a decanter
centrifuge and the liquid screened with an 80-mesh screen. Liquid
extract was concentrated in an evaporator to obtain 29.60 kgs at
21.50% solids. The concentrate was checked for solids. Maltodextrin
(M510) was then added in an amount equal to 50% of the solids level
in the concentrate. For example, 29.60 kg concentrate.times.21.50%
solids=6.36 kg solids. 6.36 kg solids.times.50%=3.18 kg
maltodextrin added. (See Table 4, line 1) The pH was 4.7. The
concentrate was spray dried in a spray dryer to yield only 56.04%
powder. ([5.35 kg after spray drying/(6.36 kg total solids+3.18 kg
carrier)].times.100=56%). The powder was very sticky, did not flow
at all, and yielded only 5.35 kgs. The ratio of root to spray dried
powder was 9.35:1.
EXAMPLE 2
[0051] Echinacea purpurea root
[0052] Alcohol to root ratio: 10:1
[0053] Temperature: heated (60.degree. C./140.degree. F.)
[0054] (See Table 4, line 2).
[0055] Batches of 50 kg of root (tea cut) were used. The alcohol to
root ratio was 10:1, and the concentration of the alcohol used was
70% (70% EtOH and 30% water). The alcohol was heated to 60.degree.
C. before the 50 kgs of root were introduced. The 50 kgs of root
were introduced into the tank through the manhole. Once the raw
material was batched into the tank with 70% EtOH/30% H.sub.2O, a
2-hour extraction was started after reaching the desired
temperature of 60.degree. C. Samples were taken at 15-minute
intervals to check soluble solids level.
[0056] Mass Balance: 50 kgs+391 kgs ethanol (200 proof)+150 kgs
H.sub.2O=518.2 kgs extract+73.1 kgs Cake (1.86% solids) (58% to 60%
moisture)
[0057] The solids were separated from the liquid in a decanter
centrifuge and the liquid screened through an 80-mesh screen.
Liquid extract was concentrated in an evaporator to obtain 42 kgs
at 23% solids. The concentrate was checked for solids, and
maltodextrin (M510) was added in an amount equal to 50% of the
solids level in the concentrate. The pH was 5.1. The concentrate
was spray dried to yield 76.05%.
EXAMPLE 3
[0058] Echinacea angustifolia root
[0059] Alcohol to root ratio: 10:1
[0060] Temperature: unheated (ambient)
[0061] (See Table 4, line 3)
[0062] Batches of 50 kg of root (tea cut) were used. The alcohol to
root ratio was 10:1, and the concentration of the alcohol used was
70% (70% EtOH and 30% water). The alcohol was unheated. The 50 kgs
of root were introduced into the tank through the manhole. Once the
raw material was batched into the tank with 70% EtOH/30% H.sub.2O,
a 2-hour extraction was started. Samples were taken at 15-minute
intervals to check soluble solids level.
[0063] Mass Balance: 50 kgs+391 kgs Ethanol (200 proof)+150 Kgs
Water=492.9 kgs of Extract+98.1 kgs of Cake (1.78% soluble solids)
(63 to 65% moisture)
[0064] The solids were separated from the liquid in a decanter
centrifuge and the liquid screened through an 80-mesh screen.
Liquid extract was concentrated in an evaporator to obtain 49 kgs
at 18% solids. The concentrate was checked for solids, and
maltodextrin (M510) was added in an amount equal to 50% of the
solids level in the concentrate. The pH was 4.7. The concentrate
was spray dried to yield 81.03%.
EXAMPLE 4
[0065] Echinacea angustifolia root
[0066] Alcohol to root ratio: 10:1
[0067] Temperature: heated (60.degree. C./140.degree. F.)
[0068] (See Table 4, line 4)
[0069] Batches of 50 kg of root (tea cut) were used. The alcohol to
root ratio was 10:1, and the concentration of the alcohol used was
70% (70% EtOH and 30% water). The alcohol was heated to 60.degree.
C. before the 50 kgs of root were introduced. The 50 kgs of root
were introduced into the tank through the manhole. Once the raw
material was batched into the tank with 70% EtOH/30% H.sub.2O, a
2-hour extraction was started after reaching the desired
temperature of 60.degree. C. Samples were taken at 15-minute
intervals to check soluble solids level.
[0070] Mass Balance: 50 kgs+391 kgs Ethanol (200 proof)+150 Kgs
Water=520.8 kgs of Extract+70.2 kgs of Cake (2.40% soluble solids)
(56 to 60% moisture)
[0071] The solids were separated from the liquid in a decanter
centrifuge and the liquid was screened through an 80-mesh screen.
Liquid extract was concentrated in an evaporator to obtain 48.5 kgs
at 26% solids. The concentrate was checked for solids, and
maltodextrin (M510) was added in an amount equal to 50% of the
solids level in the concentrate. The pH was 5.1. The concentrate
was spray dried to yield 89.00%.
EXAMPLE 5
[0072] Echinacea purpurea root
[0073] Alcohol to root ratio: 7:1
[0074] Temperature: unheated (ambient)
[0075] (See Table 4, line 5)
[0076] Batches of 50 kg of root (tea cut) were used. The alcohol to
root ratio was 7:1, and the concentration of the alcohol used was
70% (70% EtOH and 30% water). The alcohol was unheated. The 50 kgs
of root were introduced into the tank through the manhole. Once the
raw material was batched into the tank with 70% EtOH/30% H.sub.2O,
a 2-hour extraction was started. Samples were taken at 15-minute
intervals to check soluble solids level.
[0077] Mass Balance: 50 kgs+391 kgs Ethanol (200 proof)+150 Kgs
Water=493.0 kgs of Extract+98.0 kgs of Cake (1.21% soluble solids)
(60 to 65% moisture)
[0078] The solids were separated from the liquid in a decanter
centrifuge, and the liquid was screened through an 80-mesh screen.
Liquid extract was concentrated in an evaporator to obtain 26.0 kgs
at 23% solids. The concentrate was checked for solids, and
maltodextrin (M510) was added in an amount equal to 50% of the
solids level in the concentrate. The pH was 4.7. The concentrate
was spray dried to yield 66.50% .
EXAMPLE 6
[0079] Echinacea purpurea root
[0080] Alcohol to root ratio: 7:1
[0081] Temperature: heated (60.degree. C./140.degree. F.)
[0082] (See Table 8, line 6)
[0083] Batches of 50 kg of root (tea cut) were used. The alcohol to
root ratio was 7:1, and the concentration of the alcohol used was
70% (70% EtOH and 30% water). The alcohol was heated to 60.degree.
C. before the 50 kgs of root were introduced. The 50 kgs of root
were introduced into the tank through the manhole. Once the raw
material was batched into the tank with 70% EtOH/30% H.sub.2O, a
2-hour extraction was started after reaching the desired
temperature of 60.degree. C. Samples were taken at 15-minute
intervals to check soluble solids level.
[0084] Mass Balance: 50 kgs+391 kgs Ethanol (200 proof)+150 Kgs
Water=509.0 kgs of Extract+82.0 kgs of Cake (1.25% soluble solids)
(58 to 60% moisture)
[0085] The solids were separated from the liquid in a decanter
centrifuge and the liquid was screened through an 80-mesh screen.
Liquid extract was concentrated in an evaporator to obtain 27.76
kgs at 23% solids. The concentrate was checked for solids, and
maltodextrin (M510) was added in an amount equal to 50% of the
solids level in the concentrate. The pH was 5.1. The concentrate
was spray dried to yield 84.44% .
EXAMPLE 7
[0086] Echinacea angustifolia root
[0087] Alcohol to root ratio: 7:1
[0088] Temperature: unheated (ambient)
[0089] (See Table 4, line 7)
[0090] Batches of 50 kg of root (tea cut) were used. The alcohol to
root ratio was 7:1, and the concentration of the alcohol used was
70% (70% EtOH and 30% water). The alcohol was unheated. The 50 kgs
of root were introduced into the tank through the manhole. Once the
raw material was batched into the tank with 70% EtOH/30% H.sub.2O,
a 2-hour extraction was started. Samples were taken at 15-minute
intervals to check soluble solids level.
[0091] Mass Balance: 50 kgs+391 kgs Ethanol (200 proof)+150 Kgs
Water=489.0 kgs of Extract+102.0 kgs of Cake (1.076% soluble
solids) (64 to 66% moisture)
[0092] The solids were separated from the liquid in a decanter
centrifuge, and the liquid was screened through an 80-mesh screen.
Liquid extract was concentrated in an evaporator to obtain 22.80
kgs at 23% solids. The concentrate was checked for solids, and
maltodextrin (M510) was added in an amount equal to 50% of the
solids level in the concentrate. The pH was 4.7. The concentrate
was spray dried to yield 51.05% . The material was of poor quality.
It was light and fluffy, and also stuck to the spray dryer.
EXAMPLE 8
[0093] Echinacea angustifolia root
[0094] Alcohol to root ratio: 7:1
[0095] Temperature: heated (60.degree. C./140.degree. F.)
[0096] (See Table 4, line 8)
[0097] Batches of 50 kg of root (tea cut) were used. The alcohol to
root ratio was 7:1, and the concentration of the alcohol used was
70% (70% EtOH and 30% water). The alcohol was heated to 60.degree.
C. before the 50 kgs of root were introduced. The 50 kgs of root
were introduced into the tank through the manhole. Once the raw
material was batched into the tank with 70% EtOH/30% H.sub.2O, a
2-hour extraction was started after reaching the desired
temperature of 60.degree. C. Samples were taken at 15-minute
intervals to check soluble solids level.
[0098] Mass Balance: 50 kgs+391 kgs Ethanol (200 proof)+150 Kgs
Water=519.0 kgs of Extract+72.0 kgs of Cake (2.3% soluble solids)
(58 to 60% moisture)
[0099] The solids were separated from the liquid in a decanter
centrifuge, and the liquid was screened through an 80-mesh screen.
Liquid extract was concentrated in an evaporator to obtain 53.00
kgs at 22.5% solids. The concentrate was checked for solids, and
maltodextrin (M510) was added in an amount equal to 50% of the
solids level in the concentrate. The pH was 5.1. The concentrate
was spray dried to yield 87.77% .
[0100] The results from Examples 1-8 are shown in Table 4 in lines
1-8, respectively.
4TABLE 4 B C D Alcohol Extraction Kgs after E F G H I A to Root
Temp- Con- % Solids in Kgs Solids in Solids Ratio Kgs of Kgs after
J Example Herb Ratio erature centration Concentrate Concentrate
Heated/Unheated Carrier Spray drying % Yield Number A B C D E F G H
I J 1 E. purpurea 10:1 Ambient 29.60 21.50 6.36 1.00 3.18 5.35
56.1% 2 E. purpurea 10:1 60 C./140 F. 42.00 23.00 9.66 1.52 4.83
11.02 76.0% 3 E. angustifolia 10:1 Ambient 49.00 18.00 8.82 1.00
4.41 10.72 81.0% 4 E. angustifolia 10:1 60 C./140 F. 48.50 26.00
12.61 1.43 6.31 16.83 89.0% 5 E. purpurea 7:1 Ambient 26.00 23.00
5.98 1.00 2.99 5.965 66.5% 6 E. purpurea 7:1 60 C./140 F. 27.76
23.00 6.38 1.07 3.19 8.087 84.4% 7 E. angustifolia 7:1 Ambient
22.88 23.00 5.26 1.00 2.63 4.03 51.1% 8 E. angustifolia 7:1 60
C./140 F. 53.00 22.50 11.93 2.27 5.96 15.70 87.8%
[0101] Table 4 is shows yields for the various Echinacea
extractions described in examples 1-8.
[0102] The Column labeled "Example Number" numbers the rows in the
table to correspond with the example numbers in the specification.
For example, row 1 corresponds to Example 1. Column A, labeled
"Herb," indicates which herb was used in the extraction, Echinacea
purpurea or Echinacea angustifolia.
[0103] Column B, labeled "Alcohol to Root Ratio," indicates the
alcohol to ratio use in the extraction, either 10:1 or 7:1.
[0104] Column C, labeled "Extraction Temperature," indicates the
temperature at which the extraction was carried out, either ambient
temperature or 60 C./140 F.
[0105] Column D, labeled "Kgs after Concentration," indicates the
total mass of the concentrated liquid extract.
[0106] Column E, labeled "% Solids in Concentrate," indicates the
percentage of soluble solids present in the concentrated liquid
extract. The percentage of soluble solids is determined by
measuring the refractive index of the concentrated liquid
extract.
[0107] Column F, labeled "Kgs Solids in Concentrate," indicates the
mass of soluble solids in the concentrated liquid extract. The mass
of the soluble solids is calculated by multiplying the "Kgs after
Concentration" from Column D by the "% Solids in Concentrate" from
Column E, and dividing by 100. For example, in row 1, (29.60 Kgs of
extract)(21.50% solids)/100=6.36 Kgs solids.
[0108] Column G, labeled "Solids Ratio Heated/Unheated," indicates
the ratio of "Kgs Solids in Concentrate" from Column F for each
pair of examples (pairs are 1 and 2; 3 and 4; 5 and 6; 7 and 8)
comparing the heated extraction to the unheated extraction. In each
case, the "Kgs Solids in Concentrate" for the unheated or ambient
extraction is set at one (1). In other words, the "Kgs Solids in
Concentrate" for each unheated extraction divided by itself equals
one (1). The "Solids Ratio Heated/Unheated" for the heated
extraction is calculated by dividing the "Kgs Solids in
Concentrate" for the heated extraction by the "Kgs Solids in
Concentrate" for the unheated extraction in the same pair to
produce a ratio. For example, in row 2, (9.66 Kgs Solids in
Concentrate (Heated Extract Example 2))/(6.36 Kgs Solids in
Concentrate (Unheated Extract Example 1))=1.52.
[0109] Column H, labeled "Kgs Carrier," indicates the mass of the
carrier, in this case, Maltodextrin, that is added to the extract
prior to spray drying. Maltodextrin (M510) is added in an amount
equal to 50% of the solids level in the concentrate. The amount of
carrier added is calculated by dividing the "Kgs Solids in
Concentrate" from Column F by two (2). For example, in row 1, the
"Kgs Solids in Concentrate" from Column F is 6.36 Kgs. (6.36 Kgs
Solids in Concentrate)/2=3.18 Kgs. In this example, Maltodextrin is
added in an amount equal to half of the level of solids, or 3.18
Kgs Maltodextrin is added.
[0110] Column I, labeled "Kgs after Spray Drying," indicates the
yielded mass in Kgs of the solids after spray drying. The mass
after spray drying includes the mass of the soluble solids and the
mass of carrier added before spray drying.
[0111] Column J, labeled "% Yield," indicates the percentage of
soluble solids yielded relative to the total mass of solids after
spray drying. The "% Yield" is calculated by dividing the "Kgs
after Spray Drying" from Column I by the sum of "Kgs Solids in
Concentrate" from Column F and "Kgs Carrier" from Column H. The
result is then multiplied by 100 to give a percentage. For example,
in row 1, [(5.35 Kgs after spray drying)/(6.36 Kgs solids in
concentrate)+(3.18 Kgs carrier)].times.100=56.1%.
[0112] Column K, labeled "Kgs Herb for 1 Kg Powder," indicates the
mass of the raw herb starting material required to yield 1 Kg of
the extract powder. "Kgs Herb for 1 Kg Powder" is calculated by
dividing the mass of the raw starting material, by the "Kgs after
Spray Drying" from Column I. The mass of the raw starting material
is 50 Kgs for each of the examples, 1-8. For example, in row 1, (50
Kgs starting material)/(5.35 Kgs after spray drying)=9.34 Kg root
to make 1 Kg extract.
[0113] Column L, labeled "Powder Evaluation," relates to the
evaluation of the spray dried powder in terms of its moisture
uptake and flow characteristics. The two entries for Column L are
"A" and "B." "A" indicates that the powder had better tableting
characteristics and lower moisture uptake. "B" indicates that the
powder does not flow well.
[0114] Column M, labeled "% Alkylamides," indicates the percentage
of the alkylamide marker compounds in each of the spray dried
powders.
[0115] As illustrated by comparing the pairs of numbers in Column
G, for each pair of extractions, the heated alcohol extraction
yielded more soluble solids than the unheated extraction. As shown
in Column J, the percent yield was also higher for each heated
extract compared to its unheated pair. Consequently, as illustrated
in Column K, for each pair, significantly less raw herb root is
required to produce a given amount of spray dried extract for the
heated extractions compared to the unheated extractions.
[0116] The experiments above show that by using a heated alcohol
extraction process with a 10:1 alcohol to root ratio according to
the present invention, the extraction yields up to 50% more soluble
solids and high levels of nutrients or marker compounds than
conventional extraction methods.
[0117] By using the methods of the present invention, there is a
greater yield of powder when the alcohol/water solvent mixture is
evaporated off the liquid extract. A greater yield from a given
amount of starting material means that the process is economically
more efficient than traditional ambient temperature alcohol/water
extractions. In both cases, using Echinacea purpurea and Echinacea
angustifolia, the product not only was produced more efficiently
and at a lower cost, but also with a higher level of the marker
compounds, alkylamides.
[0118] In summary, there are numerous advantages to using the
extraction methods of the present invention. These extraction
methods produced 40% to 50% more soluble solids, concentrated well,
and spray dried (with M510-Maltodextrin) at a higher efficiency to
produce a better (non-sticking, low moisture uptake) spray dried
powder.
[0119] Although the description above contains many specifics,
these should not be construed as limiting the scope of the
invention, but as merely providing illustrations of some of the
presently preferred embodiments of this invention. Thus the scope
of this invention should be determined by the appended claims and
their legal equivalents, rather than by the examples given.
* * * * *