U.S. patent application number 10/221126 was filed with the patent office on 2004-02-12 for tobacco treatment.
Invention is credited to Anderson, Ian Geoffrey Marchmont, Manson, Andrew John, McAdam, Kevin Gerard, O'Reilly, David.
Application Number | 20040025891 10/221126 |
Document ID | / |
Family ID | 26243823 |
Filed Date | 2004-02-12 |
United States Patent
Application |
20040025891 |
Kind Code |
A1 |
McAdam, Kevin Gerard ; et
al. |
February 12, 2004 |
Tobacco treatment
Abstract
The invention relates to a method of treating tobacco to reduce
or eliminate nitrosamines therefrom. The method comprises the use
of a supercritical fluid extraction medium at elevated temperature
and pressure to selectively remove nitrosamines compared with
nicotine removal. The nitrosamnine content for all tobacco types
can be reduced.
Inventors: |
McAdam, Kevin Gerard;
(Southampton, GB) ; Anderson, Ian Geoffrey Marchmont;
(Southampton, GB) ; Manson, Andrew John; (London,
GB) ; O'Reilly, David; (Southampton, GB) |
Correspondence
Address: |
John F Salazar
Middleton Reutlinger
2500 Brown & Williamson Tower
Louisville
KY
40202
US
|
Family ID: |
26243823 |
Appl. No.: |
10/221126 |
Filed: |
September 9, 2002 |
PCT Filed: |
March 6, 2001 |
PCT NO: |
PCT/GB01/00945 |
Current U.S.
Class: |
131/297 |
Current CPC
Class: |
A24B 15/245 20130101;
A24B 15/24 20130101 |
Class at
Publication: |
131/297 |
International
Class: |
A24B 015/24 |
Foreign Application Data
Date |
Code |
Application Number |
Mar 10, 2000 |
GB |
0005665.5 |
May 20, 2000 |
GB |
0012111.1 |
Claims
1. A tobacco treatment process wherein tobacco is subjected to
treatment with a supercritical fluid extraction medium to extract
nitrosamines from said tobacco.
2. A process according to claim 1, whereby said nitrosamines are
separated from said supercritical fluid extraction medium by
subjecting said extraction medium to a nitrosamine removal
process.
3. A process according to claim 2, wherein said nitrosamine removal
process comprises a chemisorption step.
4. A process according to claim 3, wherein said chemisorption step
comprises the use of an ion exchanger.
5. A process according to claim 2, wherein said nitrosamine removal
process comprises an adsorbent step.
6. A process according to claim 5, wherein an adsorbent of said
adsorbent step is selected from one or more of the group consisting
of glass beads, activated charcoal, aluminium silicate and
zeolites.
7. A process according to claim 2, wherein said nitrosamine removal
process comprises treatment of said extraction medium with
ultraviolet (UV) light.
8. A process according to claim 2, wherein said nitrosamine removal
process comprises either precipitation of said nitrosamines from
said extraction medium, or subjecting said extraction medium to
nitrosamine-specific enzyme breakdown, or chromatographic
separation of said nitrosamines from said extraction medium.
9. A process according to any one of claims 2-8, wherein said
nitrosamine removal process comprises a plurality of removal
processes.
10. A process according to any one of claims 2-9, wherein following
said nitrosamine removal process, said extraction medium, being
wholly or substantially free of said nitrosamines, is brought into
contact with the tobacco, such that extract(s) other than
nitrosamines in said extraction medium may be incorporated or
re-incorporated with said tobacco.
11. A process according to claim 10, wherein said extract(s)
comprise nicotine and/or flavour substances.
12. A process according to any one of the preceding claims wherein
said supercritical fluid extraction medium is supercritical carbon
dioxide.
13. A process according to any one of the preceding claims, wherein
an acid is added to said tobacco prior to treatment of said tobacco
with said supercritical fluid; or to said supercritical fluid prior
to treatment of said tobacco with said supercritical fluid.
14. A process according to any one of claims 4 or 5 when appended
to claim 3, wherein an acid is added to the ion exchanger or
adsorbent.
15. A process according to any one of claims 1-14, wherein one or
more of an organic solvent or an alcohol is added in addition to,
or alternatively of, said acid.
16. A process according to claim 15, wherein said acid is an
organic acid.
17. A process according to claim 16, wherein said acid is an
organic acid selected from one or more of the group consisting of
malonic acid, ascorbic acid, succinic acid, glutanic acid, adipic
acid, malic acid, tartaric acid, mucic acid and citric acid, or a
salt derivative thereof.
18. A process according to claim 17, wherein said organic acid is a
citric acid salt.
19. A process according to claim 18, wherein said citric acid salt
is potassium citrate.
20. A process according to any one of the preceding claims, wherein
said extraction of said nitrosamines from said tobacco with said
supercritical fluid takes place at an elevated pressure and
temperature.
21. A process according to claim 20, wherein when supercritical
fluid is supercritical carbon dixoide, said pressure is in the
range of 100 to 350 bar.
22. A process according to claim 21, wherein said pressure is about
200 to 300 bar.
23. A process according to claim 22, wherein said pressure is about
240 to 260 bar.
24. A process according to any one of claims 20-23, wherein said
temperature is greater than about 35.degree. Celsius.
25. A process according to claim 24, wherein said temperature is an
a range of about 35.degree. to about 140+ Celsius.
26. A process according to claim 25, wherein said temperature is in
a range of about 35.degree. to about 90.degree. Celsius.
27. A process according to any one of the preceding claims, wherein
said tobacco is placed in a closable chamber or bomb during said
extraction treatment thereof with supercritical fluid.
28. A process according to any one of claims 20 to 27, wherein said
elevated temperature is effected by heat transfer or by
electromagnetic radiation.
29. A process according to any one of the preceding claims wherein
no, or very little, nicotine is removed from said tobacco in said
extraction medium.
30. A process according to any one of the preceding claims, wherein
the pH of said tobacco is less than about 6.5.
31. A process according to claim 30, wherein said pH of said acid
is less than about 5.5.
32. A process according to any one of the preceding claims, wherein
the ratio of the percentage reduction in nitrosamines to the
percentage reduction in nicotine is in the range of about 1.1:1 to
about 18:1.
33. A process according to claim 32, wherein said ratio is in the
range of about 1.3:1 to about 10:1.
34. A process according to claim 33, wherein said ratio is in the
range of about 2:1 to about 6:1.
35. A process according to any one of the preceding claims, wherein
a suitable mass flow rate of said supercritical fluid extraction
medium per kg of tobacco is about 1-55 kg/h.
36. A process according to claim 35, wherein said mass flow rate is
in the range of 10-40 kg/hr.
37. A process according to claim 36, wherein said mass flow rate is
in the range of 15-35 kg/hr.
38. A process according to claim 37, wherein said mass flow rate is
about 30 kg/h.
39. A process according to any one of the preceding claims, wherein
said tobacco treated in accordance with said process is cut tobacco
and/or whole leaf tobacco, tobacco dust or reconstituted
tobacco.
40. A process according to any one of the preceding claims, wherein
said tobacco is subjected to a microbial deactivation process.
41. A process according to claim 40, wherein said microbial
deactivation process comprises a pasteurisation process.
42. A process according to claim 41, wherein said tobacco is heated
to a temperature in the range of about 70.degree. C. to about
150.degree. C. for a period of between 30 seconds to 2 minutes.
43. A process according to claim 41, wherein said pasteurisation
process is effected by heating of said tobacco by convection
heating by way of contacting said tobacco with a gaseous heating
medium, by microwave heating or by radio frequency heating.
44. A process according to any one of claims 40-43, wherein the
moisture content of said tobacco being subjected to said microbial
deactivation process is adjustable by way of either a pre- or
post-conditioning step.
45. A process according to claim 41, wherein said microbial
deactivation process comprises use of ionising radiation, UW
radiation, freeze drying or an electron beam.
46. A process according to any one of claims 1-45, wherein said
tobacco is subjected to nitrite/nitrate removal process, before,
during or after treatment of said tobacco with said supercritical
fluid.
47. A process according to claim 46, wherein said nitrite/nitrate
removal process comprises the steps of solvent extraction to remove
nitrites/nitrates from said tobacco followed by ion exchange to
bind said nitrites/nitrates.
48. A process according to claim 46, wherein said nitrite removal
process comprises an oxidation step or use of micro-organisms.
49. A process according to any one of claims 46-48, wherein
ascorbic acid is applied to said tobacco, incorporated with said
supercritical fluid, or incorporated with a chemisorption
medium.
50. A nitrosamine extraction apparatus in use according to any one
of the preceding claims, said apparatus being a closed system
comprising a first chamber for the treatment of said tobacco with
supercritical fluid, a second chamber in which said nitrosamine
removal process takes place, said chambers being interconnected by
interconnecting means, said apparatus further comprising
supercritical fluid supply means supplying supercritical fluid,
fluid transfer means operable to cause said supercritical fluid to
flow around said closed system, and a nitrosamine removal material
residing in said second chamber.
51. Apparatus according to claim 50, wherein said fluid transfer
means is a pump.
52. Apparatus according to claim 50, wherein said fluid transfer
means is a pressure differential system.
53. Apparatus according to any one of claims 50-52, wherein a
plurality of interconnected chambers are provided for said
treatment of said tobacco with supercritical fluid and/or a
plurality of interconnected chambers are provided for said
nitrosamine removal process.
54. Apparatus according to claim 53, wherein said supercritical
fluid flows sequentially through said chambers.
55. A nitrosamine extraction apparatus in use according to any one
of claims 1-49, said apparatus being a closed system, wherein said
closed system comprises a chamber having inlet and outlet means
connected by interconnecting means, fluid transfer means and
nitrosamine removal means.
56. Apparatus according to claim 55, wherein said nitrosamine
removal means comprises an ion exchanger or an adsorbent held in a
supercritical fluid permeable container within said chamber.
57. A closed system according to claim 56, wherein said
interconnecting means serve for the transfer of supercritical fluid
extraction medium under the action of fluid transfer means, from
said outlet means of said chamber and through a nitrosamine removal
process station to said inlet means of said chamber.
58. A Burley tobacco having an initial nitrosamine content after
curing in the range of about 0.3 ppm--about 3.0 ppm, wherein said
Burley tobacco has a nitrosamine content that is at least 45% lower
following treatment according to the process of any one of claims
1-49.
59. A Virginia tobacco having an initial nitrosamine content after
curing less than 8.5 ppm, wherein said Virginia tobacco has a
nitrosamine content that is at least 45% lower following treatment
according to the process of any one of claims 1-49.
60. A Burley or Virginia tobacco according to claim 59 or 60,
wherein said nitrosamine content is at least 60% lower than the
original content.
61. A Burley tobacco having an initial nitrosamine content of 5-6
ppm, the nitrosamine content after treatment according to any one
of claims 1-49 being 3.6 ppm or less.
62. A US blended tobacco having an original nicotine content in the
range of 0.10-2.0% and a nitrosamine content in the range of 0.10-0
1.2 .mu.g/g, wherein said blend after processing according to any
one of claims 1-49 has a ratio of percentage decrease in
nitrosamines to percentage decrease in nicotine in the range of 1:1
to 10:1.
63. A Virginia tobacco blend having an original nicotine content in
the range of 0.10-2.0% and a nitrosamine content in the range of
0.10-1.2 .mu.g/g, wherein said blend after processing according to
any one of claims 1-49 has a ratio of percentage decrease in
nitrosamine to percentage decrease in nicotine in the range of 1:1
to 10:1.
64. A tobacco blend according to claim 62 or 63, wherein said ratio
is preferably 5:1 or more.
65. A tobacco blend according to claim 62 or 63, wherein said ratio
is preferably 8:1 or more.
66. A tobacco treatment process substantially as hereinabove
described with reference to FIGS. 1 and 2 hereof.
Description
[0001] The present invention relates to a method of treating
tobacco to reduce or eliminate the content of nitrosamines therein,
particularly tobacco specific nitrosamines,
[0002] Tobacco specific nitrosamines include N'-nitrosonornicotine,
4-(methylnitrosamino)-1-(3-pyridyl)-1-butanone, N'-nitrosoanatabine
and N'-nitrosoanabasine.
[0003] Various methods are known for the removal of nitrosamines
from tobacco. In U.S. Pat. No. 5,803,081 and WO 98/58555 green leaf
tobacco (i.e. tobacco prior to curing) is subjected to microwave
radiation, convection heating or freeze drying in order to kill
microbes thought to be responsible for the production of
nitrosamines during curing of the tobacco. A disadvantage of this
method is that the method includes the requirement of specific
curing practices for the tobacco, which curing practices are
carried out on the tobacco at an early stage post-harvest.
[0004] An aim of the present invention is to provide an improved
method for reducing nitrosamines in tobacco.
[0005] A further aim of the present invention is to provide an
improved method for selectively reducing nitrosamines in
tobacco.
[0006] The present invention provides a tobacco treatment process
wherein tobacco is subjected to treatment with a supercritical
fluid extraction medium to extract nitrosamines from said
tobacco.
[0007] Preferably, nitrosamines are separated from the
supercritical fluid extraction medium by subjecting the extraction
medium to a nitrosamine removal process.
[0008] Suitably, the nitrosamine removal process may comprise a
chemisorption step. Preferably, the chemisorption step may comprise
the use of an ion exchanger.
[0009] Alternatively, the nitrosamine removal process may comprise
an adsorbent step. A suitable adsorbent may be selected from one or
more of the group consisting of glass beads, activated charcoal,
aluminium silicate and zeolites. Other suitable adsorbents known to
those persons skilled in the art may also be used.
[0010] In a further alternative, the nitrosamine removal process
may comprise treatment of the extraction medium with ultraviolet
(UV) light, resulting in the breakdown of nitrosamines in the
extraction medium.
[0011] Yet further alternatives include the removal of nitrosamines
by precipitating the nitrosamines from the extraction medium; by
subjecting the extraction medium to nitrosamine specific enzyme
breakdown; or by chromatographic or other methods of separation
known to those persons skilled in the art.
[0012] The process for nitrosamine removal from the extraction
medium may comprise more than one of the above outlined nitrosamine
removal processes. In certain circumstances, at least, use of a
plurality of removal processes (together comprising a
multi-process) will result in an enhanced specificity of removal of
nitrosamines. For example, the nitrosamine removal process may be a
multi-process comprising a chemisorption step in combination with
or followed by treatment with UV light. Prior to the UV light
treatment a washing step may be required to remove the nitrosamines
from the chemisorption medium, the UV light then being applied to
the washings. Water, an acid, a salt solution or an alcohol may
suitably be used in the washing step.
[0013] Suitably, the extraction medium having had some, if not all,
of the nitrosamines removed therefrom may be brought into contact
with tobacco, such that extract(s) other than nitrosamines in the
medium may be incorporated or re-incorporated with the tobacco.
Such extract(s) may, for example, comprise nicotine and/or flavour
substances.
[0014] Much by preference, the supercritical fluid used is
supercritical carbon dioxide, although other supercritical fluids
known to the skilled person may be suitable.
[0015] Suitably, an acid, preferably an organic acid, may be added
to the tobacco prior to treatment of the tobacco with supercritical
fluid. Alternatively, the acid may be incorporated with the
supercritical fluid. Furthermore, when an ion exchanger or
adsorbent material is present, the acid may be incorporated with
the ion exchanger or adsorbent. A suitable acid may be an organic
acid selected from one or more of the group consisting of malonic
acid, ascorbic acid, succinic acid, glutaric acid, adipic acid,
malic acid, tartaric acid, mucic acid and citric acid, or a salt
derivative(s) thereof. Preferably, the organic acid is a citric
acid salt, potassium citrate for example. Other suitable acids may
be mineral acids, for example sulphuric acid and phosphoric acid.
Suitably, when the acid is applied to the tobacco the acid is in
solution. Such solution may be applied by spraying. Advantageously,
the application of the acid to the tobacco may take place in a
casing cylinder conventionally used within the tobacco industry for
applying casings to tobacco.
[0016] Other modifiers, such as organic solvents or alcohols, for
example, may alternatively or additionally be used.
[0017] Preferably, the extraction treatment of the tobacco with the
supercritical fluid takes place at an elevated pressure and
temperature. Suitably, when the supercritical fluid is carbon
dioxide a pressure in the range of 100 to 350 bar may be used,
preferably the pressure being about 200 to 300 bar and more
preferably being about 240 to 260 bar. Preferably, the temperature
used is greater than about 350 Celsius, more preferably in a range
of about 35 to about 140.degree. Celsius, and even more preferably
in a range of about 35 to about 90.degree. Celsius.
[0018] Advantageously, the tobacco is placed in a closable chamber
or bomb during the extraction treatment thereof with the
supercritical fluid.
[0019] Heating may be effected by heat transfer or by
electromagnetic radiation (i.e. microwave or radiofrequency
heating). When electromagnetic radiation is used the closed chamber
or bomb will, of course, have to be made of a non-electromagnetic
absorbing material, e.g. non-metallic material, capable of
withstanding the operating pressure. A suitable such material may
be comprised of a polyfluorohydrocarbon material, such as Teflon
(Trademark) for instance.
[0020] The technical effect of removing tobacco specific
nitrosamines by processing of tobacco with supercritical fluid was
heretofore unknown. Much by preference the conditions at which the
extraction treatment of the tobacco with the supercritical fluid
takes place are biased towards extraction in the supercritical
fluid of nitrosamines, as compared with other tobacco specific
compounds, such as nicotine for instance. Advantageously, no or
very little, nicotine is removed from the tobacco in the extraction
medium. Conditions which favour nitrosamine extraction (compared
with nicotine extraction) include a pH of the tobacco of less than
about 6.5, and preferably less than about 5.5.
[0021] Preferably, the ratio of the percentage reduction in
nitrosamines to the percentage reduction in nicotine in tobacco,
which tobacco has been subjected to the process of the present
invention, is in the range of about 1.1:1 to about 18:1, more
preferably about 1.3:1 to about 10:1, and even more preferably
about 2:1 to about 6:1.
[0022] For a given set of treatment conditions, including, for
example, the mass flow rate of the extraction medium per unit mass
of the tobacco, there will occur, after the elapse of a time
interval from commencement of the treatment process, a maximum
difference between the extraction of the (greater) percentage
amount of nitrosamines and the (lesser) percentage amount of
nicotine. Thus it may be preferable to discontinue the extraction
treatment at or about this time.
[0023] A suitable mass flow rate of the supercritical fluid
extraction medium per kg of tobacco is in the range of about 1 kg/h
to about 55 kg/h, and is dependent on the process conditions, such
as the tobacco packing density in the chamber and the size of the
chamber. Advantageously the mass flow rate of the supercritical
fluid extraction medium per kg of tobacco is in the range of 10 to
40 kg/h, more advantageously is in the range of 15 to 35 kg/h and
is even more advantageously about 30 kg/h, although these figures
do depend on what the desired product characteristics are.
[0024] Advantageously, the tobacco treated in accordance with the
process of the present invention is cut tobacco, being cut lamina
and/or cut stem tobacco. Alternatively, or in addition, the tobacco
may be one or more of whole leaf tobacco, tobacco dust and
reconstituted tobacco.
[0025] If deemed appropriate, the tobacco treated in accordance
with the process of the present invention may be subjected to a
conditioning step, whereby the moisture content of the tobacco,
post-treatment, is brought to less than about 15%, preferably less
than 13%.
[0026] When it is the case that following treatment of tobacco with
the supercritical fluid, the nitrosamines are separated from the
supercritical fluid extraction medium by subjecting the medium to a
nitrosamine removal process, preferably the medium flows around a
closed system.
[0027] Suitably, the closed system may comprise a first chamber,
for the treatment of the tobacco with supercritical fluid, and a
second chamber in which the nitrosamine removal process takes
place, wherein the first and second chambers are interconnected by
interconnecting means, pipe(s) for example. Such system further
comprises fluid transfer means operable to cause the extraction
medium to flow around the closed system. A nitrosamine removal
material such as an ion-exchange resin or adsorbent may reside in
the second chamber, such that supercritical fluid extraction
medium, following treatment of the tobacco therewith, is
transferred via the interconnecting means to the second chamber,
wherein nitrosamines are totally or substantially removed. The
supercritical fluid extraction medium, minus nitrosamines, may then
be returned to the tobacco in the first chamber.
[0028] Suitably, a plurality of interconnected chambers may -be
provided for the treatment of the tobacco with supercritical fluid
and/or a plurality of interconnected chambers may be provided for
the nitrosamine removal process. When it is the case that more than
one chamber is provided for either the treatment of the tobacco or
the nitrosamine removal process, or for both, the supercritical
fluid may flow sequentially through the chambers.
[0029] Alternatively, the closed system may comprise a first or
single chamber having inlet and outlet means wherein
interconnecting means interconnect the inlet with the outlet means
of the chamber. Suitably, the interconnecting means may serve for
the transfer of supercritical fluid extraction medium, under the
action of fluid transfer means, from the outlet means of the
chamber to and through a nitrosamine removal process station to the
inlet means of the chamber. Preferably, the amount of fluid in the
interconnecting means is kept to a minimum. A nitrosamine removal
material, such as an ion exchanger or an adsorbent, may be
contained within any suitable permeable container so as to provide
a means by which fluid may pass through the container and a means
by which the tobacco is prevented from contact with the nitrosamine
removal material.
[0030] Alternatively the nitrosamine removal process may, for
instance, be constituted by the transfer of the medium through a UV
light source. In this instance, the interconnecting means must be
pervious to UW light.
[0031] Suitably, a plurality of interconnected chambers may be
provided for the treatment of the tobacco with supercritical
fluid.
[0032] In addition to subjecting the tobacco to treatment with the
supercritical fluid to extract nitrosamines from the tobacco, the
tobacco may be subjected to a microbial deactivation process. As
stated above microbes, including Enterobacter agglomerans, Bacillus
spp, Fusarium equisetti, Cladosporium cladosporoides, Altenaria
alternata and Acremonium arxii are thought to be responsible for or
contribute to the production of nitrosamines during curing of the
tobacco. In fact, it is thought that microbes may also be a
contributory factor in the production of nitrosamines in tobacco
during storage of cured tobacco. Thus a reduction in microbial
activity in the tobacco by way of the microbial deactivation
process reduces the likelihood of reformation of nitrosamines in
the tobacco post-extraction thereof. The microbial deactivation
process may be carried out before or after subjecting the tobacco
to the treatment with the supercritical fluid. A further
alternative is to subject the tobacco to treatment with the
supercritical fluid under microbial deactivating conditions, such
that microbial deactivation and extraction occur
simultaneously.
[0033] Suitably, the microbial deactivation process may comprise a
pasteurisation process, wherein the tobacco is heated to a
specified temperature and maintained at that temperature for a set
period of time. By way of example, the tobacco may be heated to a
temperature in the range of about 70.degree. to about 150.degree.
Celsius for a period of between about 30 seconds to about 2
minutes. The heating may be effected by, for example, convection
heating by way of contacting the tobacco with a gaseous heating
medium, microwave heating or radio frequency heating.
[0034] Suitably, the moisture content of the tobacco being
subjected to the sterilisation process is adjustable by way of
either a pre- or a post-conditioning step.
[0035] Alternatively, the treatment of tobacco with, for example,
ionising radiation, UV radiation, freeze drying or an electron beam
to kill microbes may be used as the microbial deactivation
process.
[0036] In addition to the treatment of the tobacco with the
supercritical fluid to extract nitrosamines from the tobacco, the
tobacco may also be subjected to a nitrite/nitrate removal process.
Nitrites are important precursors of nitrosamines, whereas nitrates
are precursors of nitrites. It is thought that following
nitrosamine removal residual nitrites in the tobacco may be free to
react with alkaloids also present in the tobacco thus to re-form
nitrosamines. The nitrite/nitrate removal process may suitably
comprise the steps of solvent extraction to remove the
nitrites/nitrates from the tobacco, followed by ion exchange to
bind the nitrites/nitrates. Alternatively, the nitrites may be
removed by way of an oxidation step. In a yet further alternative,
removal of nitrites/nitrates using micro-organisms as disclosed in
any one of GB 1 440 171, GB 1 585 024, U.S. Pat. No. 4,709,710 or
GB 2 014 031 may be used.
[0037] As with the microbial deactivation process, the
nitrite/nitrate removal process may be carried out before, after or
during the treatment of the tobacco with the supercritical fluid.
When the nitrite/nitrate removal process is carried out
simultaneously with the treatment of the tobacco with the
supercritical fluid, the process may in order to remove nitrites
from the tobacco comprise, for example, the step of either applying
ascorbic acid to the tobacco prior to treatment of the tobacco with
the supercritical fluid; incorporating ascorbic acid with the
supercritical fluid; or, when an ion exchanger or adsorbent
material is present, incorporating ascorbic acid with the ion
exchanger or adsorbent. The ascorbic acid has the effect of
scavenging nitrites from the tobacco.
[0038] The nitrite/nitrate removal process may be carried out as an
alternative to or in addition to the microbial deactivation
process.
[0039] The inventive process provides a Burley tobacco having an
initial nitrosamine content after curing in the range of about 0.3
ppm--about 30 ppm, which after processing has a nitrosamine content
that is at least 45% lower. If the tobacco is a Burley tobacco
having a nitrosamine content of 5-6 ppm, after processing the
content is preferably 3.6 ppm or less.
[0040] The inventive process also provides a Virginia tobacco
having an initial moisture content after curing of less than 8.5
ppm, which after processing has a nitrosamine content that is at
least 45% lower.
[0041] Preferably the Burley or Virginia processed tobacco have a
nitrosamine content of at least 60% lower than its original
content.
[0042] The inventive process also provides a US blended tobacco
having an original nicotine content in the range of 0.10-2.0% and a
nitrosamine content in the range of 0.10-1.2 .mu.g/g which after
processing has a percentage decrease in nitrosamines to percentage
decrease in nicotine in the range of 1:1 to 10:1.
[0043] The inventive process also provides a Virginia blended
tobacco having an original nicotine content in the range of
0.30-2.15% and a nitrosamiine content in the range of 0.10-1.5
.mu.g/g, which after processing has a percentage decrease in
nitrosamines to percentage decrease in nicotine in the range of 1:1
to 10:1.
[0044] Preferably the ratio is in the range of 5:1 or more, and
more preferably 8:1 or more.
[0045] In order that the present invention may be clearly
understood and readily carried into effect reference will now be
made, by way of example, to the accompanying diagrammatic drawing,
in which:-
[0046] FIG. 1 shows an apparatus for carrying out a process
according to a first aspect of the present invention; and
[0047] FIG. 2 shows an apparatus for carrying out a process
according to an alternative aspect of the present invention.
[0048] The apparatus as shown in FIG. 1 is a closed system
comprising a first chamber 1 and a second chamber 2 wherein the
first and second chambers 1, 2 are interconnected by
interconnecting pipes 3. The closed system further comprises fluid
transfer means, namely a pump 4. The apparatus further comprises a
reservoir tank 5 interconnected with the first chamber 1 via a duct
6. Valve 7 is located in duct 6 which valve 7 is operable to close
the tank 5.
EXAMPLE 1
[0049] In operation of the FIG. 1 apparatus, about 30 kg of cut
tobacco having a moisture content of either about 14% or 25% (see
Table 1) is placed in the first chamber 1, the chamber having a
volume of 1501. An ion exchanger, namely an acidic ion exchange
resin (as available from Bayer GmbH) having a weight of 4.4 kg, is
placed into the second chamber 2, the chamber having a volume of
1501. The ion exchanger is mixed with about 500 g of solid
potassium citrate granules. The reservoir tank 5 is charged with
carbon dioxide, which carbon dioxide is then pressurised by pump
means (not shown) and is transferred by the pump means from the
reservoir tank 5 to the first and second chambers 1, 2 and the
interconnecting pipes 3 until the requisite extraction conditions
are achieved, namely a pressure of about 250 bar and a temperature
of about 70.degree. Celsius. At this point the carbon dioxide
reservoir tank is closed by closing valve 7. The supercritical
carbon dioxide is then circulated, under the action of the pump 4,
through the first chamber 1 (and, therefore, through the tobacco
contained therein) and through the second chamber 2 (and,
therefore, through the ion exchange resin therein) via the
interconnecting pipes 3. The supercritical carbon dioxide
extraction medium is circulated about the closed system for a
period of either 1.5 hours or 3 hours. Then the first and second
chambers 1, 2 are decompressed by opening vent means (not shown)
and the chambers are opened.
[0050] The nicotine and nitrosamine contents of the thus treated
tobacco are then evaluated using suitable standard laboratory
tests.
[0051] Such a tobacco extraction process has been found to remove a
substantial proportion of tobacco specific nitrosamines from the
treated tobacco. Table 1 discloses percentage reductions in the
tobacco of both nicotine and nitrosamines following treatment of
the tobacco as outlined above. The total amount of CO.sub.2 used
for these examples was 2109 kg.
1TABLE 1 Nicotine Nitrosamines Tobacco Extraction Reduction
Reduction Run No. m.c. Period (h) (%) (%) 1 14% 1.5 67 90 2 14% 3.0
78.5 94 3 25% 1.5 65.5 93.5 4 25% 3.0 77 95
[0052] Treatment for 1.5 hours results in a greater difference
between the percentage amount of nitrosamines and the percentage
amount of nicotine extracted, as compared with treatment for 3
hours.
EXAMPLE 2
[0053] It was believed that the extraction period outlined above
could be reduced further without substantially affecting the
percentage reduction of nitrosamines, whilst further reducing the
percentage reduction of nicotine. For instance, the extraction
period may be between about 15 minutes to about 1.5 hours,
preferably between about 20 minutes to about 1 hour, more
preferably between about 25 minutes to about 40 minutes and even
more preferably about 30 minutes.
[0054] The conditions of extraction are preferably further biased
towards the extraction in the supercritical fluid of nitrosamines,
as compared with other tobacco specific compounds, such as
nicotine. Several other methods of biasing the extraction towards
nitrosamine removal, as compared with other tobacco specific
compounds, may be used in addition to or separately from adjustment
of the extraction period. For instance, the pH of the tobacco may
be maintained at less than about 6.5, preferably about 5.5. In
accordance with a further alternative, the supercritical fluid
extraction medium may be saturated, or substantially saturated,
with tobacco specific compounds, or commercially available chemical
analogues thereof, other than nitrosamines before contacting the
extraction medium with the tobacco treatment. A yet further
alternative, when the supercritical fluid is carbon dioxide, may be
to cool the tobacco to a temperature below about 35.degree. C.,
such that when the supercritical carbon dioxide is pumped into the
chamber containing the tobacco the general effectiveness of the
extraction process is reduced with preferential bias against the
removal of tobacco specific compounds other than nitrosamines.
Biasing towards the extraction of nitrosamines may also be effected
by altering (i.e. increasing) the packing density of the tobacco in
the extraction chamber.
[0055] Furthermore, biasing may be effected by altering, i.e.
lowering the mass flow rate of the supercritical fluid extraction
medium per unit mass of tobacco. For example, reducing the flow
rate of the supercritical fluid per kg of tobacco to less than 30
kg/h. Each of the above outlined methods of biasing the extraction
towards nitrosamine removal, as compared with other tobacco
specific compounds, may be carried out separately or in various
combinations with one another.
[0056] As an optional addition to the above described process, the
ion exchange resin situate in the second chamber 2, following
decompression of the closed system, is flushed or washed with
water. The washings are then treated with UV light from a UV light
source (not shown). Exposure of the washings to UV light results in
the degradation of nitrosamines in the washings. Extract(s) other
than nitrosamines in the washings is then re-incorporated with the
tobacco. Other extract(s) may include, for example, nicotine and/or
flavour substances. In this way, the end result is that
nitrosamines are selectively removed from the tobacco, without
adversely affecting the taste of the tobacco.
[0057] Some examples of the above described variations are
disclosed in Table 2 below.
[0058] In view of the variability of nicotine and nitrosamine
contents in each batch of tobacco, 300 g from each batch was
retained as a control for the batch. The nicotine and nitrosamine
levels for each control from the 4 batches sampled are given in
Table 3 below.
2TABLE 2 Total Nicotine % TSNA in Other Trial/ Tob type in blend
nicotine blend % TSNA Extraction Total process run & wt %
reduction .mu.g/g reduction time CO.sub.2 kg variables 1 run 2 238/
0.53 78.46 0.14 94.33 3 hrs 2190 15% moist 35 kg tobacco 1 run 4
238/ 0.56 77.24 0.12 95.14 3 hrs 2190 25% moist 35 kg tobacco 1 run
5 238/ 0.33 86.59 0.15 93.93 3 hrs 2190 500 g Citrate 35 kg added
to ion exchanger 1 run 7 USB/ 0.17 91.58 0.12 97.12 3 hrs 2190 15%
moist 35 kg tobacco 1 run 9 USB/ 0.14 93.07 0.20 95.20 3 hrs 2190
25% moist 35 kg tobacco 4 run 1 USB/ 1.47 20.11 1.13 61.69 2 hrs 40
At original pH 3 kg (5.44) 4 run 3 USB/ 1.7 7.61 1.08 63.39 2 hrs
40 pH of tobacco 3 kg reduced (4.1- 4.3) 4 run 4 238/ 1.96 14.78
0.72 70.49 2 hrs 40 3 kg 4 run 6 238/ 2.12 7.83 1.36 44.26 2 hrs 10
3 kg 3 run 11 238/ 2.1 8.7 0.65 73.36 15 mins 200 15 kg 5 run 3
USB/ 1.4 22.65 1.11 66.57 2.5 hrs 40 Glass beads, no 3 kg ion
exchanger
[0059]
3 TABLE 3 Nicotine Content (%) Nitrosamine Content (.mu.g/g) Batch
No. USB 238 USB 238 1 2.02 2.46 4.17 2.47 4 1.84 2.30 2.95 2.44 3
1.84 2.29 2.95 2.44 5 1.77 not 3.32 not reported reported yet
yet
EXAMPLE 3
[0060] The apparatus shown in FIG. 2 is also a closed system, which
apparatus comprises a chamber 1 provided with an inlet 8 and an
outlet 9, interconnecting pipe 10, wherein the pipe 10
interconnects the inlet 8 with the outlet 9 of the chamber 1, and
fluid transfer means, i.e. a pump 4. This apparatus further
comprises a reservoir tank 5 interconnected with the chamber 1 via
a duct 6. Valve 7 located in duct 6 allows for tank 5 to be closed.
Adjacent a position of the pipe 10 is located a UV light
source.
[0061] In operation of the FIG. 2 apparatus about 100 kg of cut
tobacco having an appropriate moisture content is placed into
chamber 1. The reservoir tank 5 is charged with carbon dioxide,
which carbon dioxide is then pressurised by pump means (not shown)
and is transferred by the pump means from the reservoir tank 5 to
the chamber 1 and pipe 10 until the requisite extraction conditions
are achieved, namely a pressure of about 250 bar and a temperature
of about 50.degree. Celsius. Then the tank 5 is closed by closing
the valve 6. The supercritical carbon dioxide is then circulated,
under the action of the pump 4, through the chamber 1 (and,
therefore, through the tobacco contained therein) and through the
pipe 10. The UV light source 11 irradiates the supercritical carbon
dioxide extraction medium in the pipe 10. Thus, nitrosamines in the
supercritical carbon dioxide are degraded. Degradation products
thereof may then be removed, for instance by passing the
supercritical carbon dioxide through a metal mesh (not shown). The
pipe 10 is comprised of, at least in the region of the UV light
source 11, material which is pervious to UV light, e.g. a high
pressure quartz window. The amount of supercritical carbon dioxide
in the interconnecting pipe 10 is kept to a minimum by use of a
pipe 10 having a bore of a small diameter (i.e. a diameter of about
1 cm). The supercritical carbon dioxide is, following exposure to
the UV light, returned to the chamber 1 and again into contact with
the tobacco therein. The supercritical carbon dioxide is circulated
for a period of 30 minutes. Then the chamber 1 and the pipe 10 are
decompressed by opening vent means (not shown). The tobacco treated
in this way is free, or substantially free, of nitrosamines, whilst
the nicotine content of the tobacco remained substantially the same
pre- and post-treatment.
[0062] A further alternative apparatus (not shown) comprises
substantially the apparatus shown in FIG. 2 with a nitrosamine
removal material held within a fluid permeable container in the
chamber 1. The fluid may be re-circulated through the system for a
number of times before removal and optional subsequent removal of
nitrosamines therefrom.
* * * * *