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Patent 2006260 Summary

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(12) Patent: (11) CA 2006260
(54) English Title: DEODORANT
(54) French Title: DESODORISANT
Status: Expired and beyond the Period of Reversal
Bibliographic Data
(51) International Patent Classification (IPC):
  • A61L 09/01 (2006.01)
(72) Inventors :
  • SAIHARA, YASUHIRO (Japan)
  • DATE, HARUYUKI (Japan)
  • YAMAUCHI, TOSHIYUKI (Japan)
  • MIZOBUCHI, MANABU (Japan)
(73) Owners :
  • MATSUSHITA ELECTRIC WORKS, LTD.
(71) Applicants :
  • MATSUSHITA ELECTRIC WORKS, LTD. (Japan)
(74) Agent: OYEN WIGGS GREEN & MUTALA LLP
(74) Associate agent:
(45) Issued: 1999-03-16
(22) Filed Date: 1989-12-20
(41) Open to Public Inspection: 1991-06-20
Examination requested: 1989-12-20
Availability of licence: N/A
Dedicated to the Public: N/A
(25) Language of filing: English

Patent Cooperation Treaty (PCT): No

(30) Application Priority Data: None

Abstracts

English Abstract


A deodorant containing deodorizing ingredients
extracted from Oleaceae family plants obtained through a
tissue culture by means of a medium with plant growth
regulators as cytokinins and/or copper ions added for a
highly efficient promotion of production of the
deodorizing ingredients within cells of the Oleaceae
family plants.


French Abstract

Divulgation d'un désodorisant contenant des ingrédients désodorisants extraits de plantes de la famille des Oleaceae obtenues par culture de tissu dans un milieu où des régulateurs de croissance des plantes comme les cytokinines et/ou des ions cuivres sont ajoutés pour une promotion des plus efficaces de la production d'ingrédients désodorisants dans les cellules des plantes de la famille des Oleaceae.

Claims

Note: Claims are shown in the official language in which they were submitted.


WE CLAIM:
1. A method for obtaining a deodorant extract from a plant
material in the family Oleaceae, which method comprises the
steps of:
(a) taking a portion of a plant of the family Oleaceae and
culturing said plant portion on a solid medium to induce the
formation of callus;
(b) transferring the resulting plant cells with induced
callus to a liquid medium which contains a cytokinin and copper
ions in an amount sufficient to increase the amount of deodorant
materials contained in the plant cells, and culturing said plant
cells in a single liquid medium stage for a time period
sufficient to increase the amount of deodorant materials
contained in the plant cells,
said cytokinin being selected from the group
consisting of N'-benzoyl adenine, 6-benzyl adenine, kinetin,
2-hydroxypurine, zeatin and mixtures thereof and being
present in the range of from 10 -7 to 10 -3M, and
said copper ions being provided by the addition of a
compound selected from the group consisting of copper
sulfate, copper nitrate, copper acetate and mixtures thereof,
in an amount of from 5 to 100 ppm on a copper sulfate
basis; and
(c) removing the plant cells from the liquid medium and
extracting the deodorant materials from the plant cells.
2. The method of claim 1, wherein the solid medium includes
agar and either an LS or Gomborg B5 medium.
3. The method of claim 1, wherein an organic and/or
inorganic acid is added to the extract obtained from step (c).
4. The method of claim 3, wherein the organic acid is
selected from the group consisting of lactic acid, succinic
acid, malic acid, tartaric acid, citric acid and mixtures
thereof, and the inorganic acid is selected from the group
consisting of phosphoric acid, boric acid, carbonic acid and
mixtures thereof.
-28-

5. The method of claim 3, wherein a pH regulator is added
to the extract obtained from step (c).
6. The method of claim 5, wherein the pH regulator is
selected from the group consisting of sodium hydroxide, potassium
hydroxide, a phosphoric acid buffer, and mixtures thereof.
7. The method of claim 1, wherein glyoxal is added to the
extract obtained from step (c).
8. The method of claim 1, wherein a surfactant is added to
the extract obtained from step (c).
9. The method of claim 1, wherein an organic acid and/or
inorganic acid, glyoxal, a surfactant, and a pH regulator which
regulates pH within the range of 3-8 is added to the extract
obtained from step (c).
10. The method of claim 9, wherein the surfactant is
selected from the group consisting of cationic and amphoteric
surfactants.
11. The method of claim 9, wherein the surfactant is
selected from the group consisting of benzalkonium chloride,
cetyl pyridinium chloride, benzetonium chloride and alkyl
polyaminoglycine.
12. The method of claim 1, wherein the Oleaceae plant is
from a genera selected from the group consisting of Osmanthus,
Forsythia, Olea, Syringa, and Fraxinus.
13. The method of claim 1, wherein the solid medium in
step (a) further includes a material selected from the group
consisting of auxins, cytokinins, and sugar.
14. The method of claim 13, wherein the amount of auxins
and cytokinins is 10 -7 to 10 -5 M, the sugar is 0 to 10 wt. %,
and the sugar is 0.7 to 20 wt. % of the solid medium.
15. The method of claim 13, wherein the auxin is selected
from the group consisting of .alpha.-naphthalene-acetic acid,
indolebutyric acid, 2,4-dichloro-phenoxyacetic acid and
mixtures thereof.
16. The method of claim 13, wherein the cytokinin is at
least one selected from the group consisting of N'-benzoyl
adenine, benzyl adenine, kinetin, 2-hydroxypurine and zeatin
and which is added to a concentration of 10 -7 to 10 -3 M.
17. The method of claim 1, wherein the liquid medium in
-29-

step (b) is White's liquid medium.
18. The method of claim 1, wherein the liquid medium of
step (b) includes the step of adding auxin at a concentration
lower than that of said cytokinins.
19. The method of claim 18, wherein the amount of auxin
is 10 -7 to 10 -3 M.
20. The method of claim 19, wherein the medium further
includes 1 to 10 wt. % of sugar.
21. The method of claim 19, wherein the auxin is selected
from the group consisting of .alpha.-naphthalene-acetic acid,
indolebutyric acid, 2,4-dichloro-phenoxy-acetic acid, and
mixtures thereof.
22. A method for obtaining a deodorant extract from a
plant material in the family of Oleaceae, which method comprises
the steps of:
(a) taking a portion of a plant of the family of Oleaceae
and culturing said plant portion on a solid medium culture bed
to induce the formation of a callus in plant cells on a
mass-production scale;
(b) transferring the resulting plant cells with said callus
induced to a liquid medium culture bed which contains a
cytokinin and copper ions in amounts effective to propagate
deodorant materials contained in the plant cells, for culturing
said plant cells in a single liquid medium stage for a time
period effective to propagate said deodorant materials contained
in the plant cells,
said-cytokinin being selected from the group consisting of
N'-benzoyl adenine, 6-benzyl adenine, kinetin, 2-hydroxypurine,
zeatin and mixtures thereof and being in the range of 10 -7 to
10 -3 M, and
said copper ion being provided by the addition of a compound
selected from the group consisting of copper sulfate, copper
nitrate, copper chloride, copper acetate and mixtures thereof
in an amount of 5 to 100 ppm on a copper sulfate basis; and
(c) removing the plant cells from the liquid from the
liquid medium culture bed, extracting the deodorant materials
from the plant cells, and adding to said deodorant material
extracted an organic acid and/or inorganic acid, glyoxal, a
-30-

surfactant, and a pH regulator which regulates pH within the
range of 3-8.
23. A method for obtaining a deodorant extract from a plant
material in the family of Oleaceae, which method comprises the
steps of:
(a) taking a portion of a plant of the family of Oleaceae
and culturing said plant portion on a solid medium to induce the
formation of callus;
(b) transferring the resultant plant cells with induced
callus to a first liquid medium selected from the group
consisting of LS medium and Comborg B5 medium;
(c) further transferring the plant cells and callus
cultured at step (b) to a second liguid medium containing a
cytokinin and copper ions in an amount sufficient to increase
the amount of deodorant materials contained in the plant cells,
and culturing said plant cells for a time period sufficient to
increase the amount of deodorant materials contained in the plant
cells,
said cytokinin being selected from the group consisting of
N'-benzoyl adenine, 6-benyl adenine, kinetin, 2-hydroxypurine,
zeatin and mixtures thereof and being present in the range of
from 10 -7 to 10 -3 M, and
said copper ions being provided by the addition of a
compound selected from the group consisting of copper sulfate,
copper nitrate, copper chloride, copper acetate and mixtures
thereof, in an amounnt of from 5 to 100 ppm on a copper sulfate
basis; and
(d) removing the plant cells from the second liquid medium
and extracting the deodorant materials from the plant cells.
24. The method of claim 23, wherein said second liquid
medium comprises an additive selected from the group consisting
of auxins, sugar and mixtures thereof, said auxins being added
to a concentration of 10 -7 to 10 -4 M and said sugar being added
in a range from 1 to 10 wt. %
25. The method of claim 24, wherein the auxin is selected
from the group consisting of .alpha.-naphthalene-acetic acid,
indolebutyric acid, 2,4-dichloro-phenoxy-acetic acid and mixtures
thereof.
-31-

Description

Note: Descriptions are shown in the official language in which they were submitted.


2006260
"DEODORANT"
SPECIFICATION
TECHNICAL BACKGROUND OF THE INVENTION
This invention relates to a deodorant which can be
mass-produced with a tissue culture employed.
The deodorant of the kind referred to is effectively
contributive to reduction of bad or offensive odors
yielded from cigarette smoke, kitchen garbage, excretion
and the like, or caused by various types of waste liquid,
exhaust gas and discharged smoke of factories, vehicles
and so on.
DESCRIPTION OF THE RELATED ART
In recent years, the offensive odors have been taken
up as an important issue of life environment contamination
and the deodorization is a great social concern, and there
have been suggested various methods for reducing the
offensive odors. First one that can be enumerated as such
methods will be a use of fragrant substance as the
deodorant for the purpose of masking human sense of smell
by means of the fragrance. However, this method is
defective in that the fragrant substance is limited in
such masking ability and, in particular, in the ability of
coping with any strong odor. Further, it is rather
difficult to balance the fragrance with the offensive
odors, and to achieve a general-purpose deodorizing action
since like and dislike vary from person to person. There
has been suggested another method, in which air in a
limited space of house room or the like is ventilated or

~ 200~iX60
diffused, but this method has been still defective in its
necessity of resorting to an expensive ventilating or the
like device, and in inherent change in the room
temperature.
Further enumerated method is a deodorization by means
of chemical reaction to ingredients of the offensive
odors, but this method requires selection of one of
different chemical substances with respect to each of
different ingredients yielding the offensive odors in
order to cause the effective chemical reaction thereto,
which results undesirably in that the selection work
becomes complicated while various sorts of deodorants must
be prepared, lowering application flexibility of the
method. With respect to the offensive odor resulting from
decomposition and the like, further methods have been
suggested for killing bacteria to cause the decomposition
to stop and to prevent the offensive odor, but they still
involve problems that expensive bactericidal apparatus is
required and it takes time until its effect appears.
Meanwhile, there has been proposed in Japanese Patent
Appln. Laid-Open Publication No. 53-66434 by J. Kawachi et
al a deodorant which requires no expensive installation
nor apparatus, and this deodorant uses active
deodorization ingredients obtained from plants and, more
specifically, contains extracts thermally extracted from
raw or dried leaves of Camellia or Cinnamomum Camphor
plant with use of organic solvent and/or water. This
deodorant is advantageous in that the use of the active

~0~ 626Q
deodorization ingredients in plants results in simple and
low cost production of the deodorant because of easy
availability of the plant, but is disadvantageous in that
the deodorizing action on the nitrogen or sulfur compound
odor is insufficient. Various prior art using the active
deodorization ingredients in plants can be seen in U.S.
Patents. No. 4,167,559 of G.M. Michel, No. 4,170,638 of
J.L. Owades, No. 4,251,508 of G.G. Monsod, Jr., and No.
4,681,757 of T. Mimasu et al, but their deodorants have
all a relatively narrow range of odor to deal with and are
poor in the application flexibility.
On the other hand, K. Osada et al have suggested
a deodorant which
realizes the deodorization with ingredients extracted from
a species of plants effective with respect to the nitrogen
or sulfur compound odor, which shows a remarkable
reduction of the offensive odor in particular of the
sulfur compound.
~ While.. the plants of such species are easily available,
they are natural plants and are limited in the growing
rate and eventually in the supply amount, so as to be
defective in that their constant supply can easily be
affected by any change in such natural environmental
conditions as wind, rain, temperature and so on.
Accordingly, the present inventors have suggested in an
earlier Japanese Patent Application No. 60-138377 a tissue
culture of plants in a genus of Forsythia showing
excellent deodorizing effect with respect to the sulfuric

2006260
.,
compound odor as well as a deodorant employing deodorizing
ingredients extracted from the plants thus cultured. The
suggested tissue culture is effective to a certain extent
to overcome the problems in the limited and unstable
supply, but it has been demanded to further improve the
efficiency in the culture and the plant supply, so as to
sufficiently maintain the supply rate of the deodorizing
ingredients.
TECHNICAL FIELD OF THE INVENTION
A primary object of the present invention is,
therefore, to provide a deodorant containing deodorizing
ingredients obtained by improving the efficiency of tissue
culture of such plants in the family of Oleaceae as
Forsythia suspensa.
Another object of the present invention is to provide
a deodorant containing deodorizing ingredients obtained at
a stable quality from the Oleaceae family plants
mass-produced.
Still another object of the present invention is to
provide a deodorant consisting of deodorizing ingredients
produced by means of a tissue culture and still
substantially of equal quality to that of extract from
natural plants.
A further object of the present invention is to
provide a deodorant capable of being used in any style of
spraying liquid, filter impregnation and solid stick.
According to the present invention, the above objects
can be realized by a deodorant containing deodorizing

Z006260
ingredients extracted from plants in the family of
Oleaceae obtained through a tissue culture with a culture
medium containing cytokinins as plant growth regulators
and copper ions.
Other objects and advantages of the present invention
shall be made clear in following explanation of the
invention detailed with reference to preferred examples.
It should be appreciated, however, that the present
invention is not to be limited only to the examples
described but is to include all modifications, alterations
and equivalent arrangements possible within the scope of
appended claims.
DISCLOSURE OF PREFERRED EMBODIMENTS
In the deodorant according to the present invention,
deodorizing ingredients extracted from the plants in the
family of Oleaceae which are obtained through a tissue
culture. For the Oleaceae family plants, there can be
employed various plants classified in such genera of the
Oleaceae family as Osmanthus, Forsythia, Olea, Syringa,
and Fraxinus. While not necessary to limit, the plants in
the genera of Osmanthus and Forsythia exhibit excellent
deodorizing effect and are preferable. In these plants of
Forsythia, further, desirable plants are Forsythia
suspensa, Forsythia japonica Makino, Forsythia Viridissima
Lindl and Forsythia koreana Nakai. There can be also
listed here as optimum plants in Osamanthus are Osmanthus
fragrans Lour. Var. Auranlacus Makino, Osamanthus fragrans
Lour. O. Asiaticus Nakai, Osmanthus heterophyllus,

2006260
Osmanthus X. Fortuneiu Carr and Osmanthus insulario
koidz.
The culture is to be carried out initially by
subjecting to bactericidal treatment such organs as
leaves, leafstalks, stalks, roots and so on of the
foregoing subject plants in a manner well known. That is,
these organs are cut into pieces of about 2 to 3cm or to
be about 2 to 3cm square, and are then sterilized by an
aqueous solution of sodium hypochlorite and ethanol.
Thereafter, they are further cut into pieces of about 1 to
2cm under sterilized condition, and are bedded on a solid
medium. Cells for the culture are subjected to an
induction of callus on a solid medium (agar), for which
medium such generally widely utilized basic medium as
Linsmaier & Skoog (LS) or Gomborg B5 or the like is used
with agar added. The thus induced callus is transplanted
to a liquid medium to carry out the tissue culture. For
the liquid medium, while not limited particularly, White's
liquid medium should preferably be employed, in view of an
excellent effect caused by inorganic components (in
particular, N components) contained in the White's medium,
due to that secondary metabolism (producing the
deodorizing ingredients) is presumably more actively
carried out than primary metabolism system of the cells
(their multiplication or growth due to production of amino
acid and the like) in this medium.
More preferable is that a suspensoid culture with the
LS or Gomborg B5 liquid medium is preliminarily carried

20(16260
out prior to the tissue culture by means of the White's
medium or the like, and the cells in logarithmic growth
phase or in stationary phase of the growth curve are
transplanted to the White's medium, for reasons that the
transplant of the cells in such phase allows the
deodorizing ingredients produced in a shorter period than
in a case of transplantation of cells in lag phase, and
that, more importantly, a larger amount of cells can be
added to the White's medium to render a larger amount of
the effective deodorizing ingredients to be eventually
obtained. It is proper that the cells thereby obtained
are added by 2-20wt.% to the White's liquid medium.
The amount of the cells contained in the medium as a
result of the transplantation is made to be 2 to 20wt.% in
fresh weight of only the cells. While the cells may be
transplanted after being separated from the medium by
means of a filtration or the like, the cells in the
suspensoid culture may be used without being separated
from the medium. In that case, the amount of the medium
of the suspensoid culture should not exceed the amount of
the White's medium of the liquid cultivation. In short,
the present invention is to be featured in such two steps
as the callus induction with the solid medium and the
tissue culture with the liquid medium for the production
of the deodorant ingredients or, more preferably, in such
three steps as the callus induction with the solid medium,
the cell growth with the suspensoid culture, and the
tissue culture with the liquid medium for producing the

2006260
deodorant ingredients.
Procedure of the tissue culture including the
induction of callus shall be further explained. While not
limited particularly, it is preferable that, to the
culture medium, such carbon source or energy source as
sugar, glucose or the like, such inorganic salts as
calcium chloride or the like, such growth factor as amino
acid, vitamins or the like are added. It is also
preferable to use in a proper combination such plant
growth regulators as auxines and cytokinins. For the
auxines, there may be enumerated ~-naphthalene-acetic
acid, indolylacetic acid, indolebutyric acid,
2,4-dichloro-phenoxyacetic acid and the like and, for the
cytokinins, N'-benzoyl adenine, benzyl adenine, Kinetin,
2-hydroxypurin, phenyl aminopurin, 6-methylpurin, zeatin
and the like may be enumerated.
In using the LS or the like solid medium (with a basic
medium of a liquid but made solid with agar added), it is
preferable to add thereto 10 to 10 5M of each of such
auxine as ~-naphthalene-acetic acid or the like and such
cytokinins as Kinetin, 0-lOwt.% (with the basic liquid
medium made as a reference) of sugar and 0.7-2.0wt.% (with
the basic liquid medium made as a reference) of agar.
After inoculation of external plant in the medium with
agar added, they are left for the culture for 2 to 3 weeks
under a normal temperature, and callus thereby produced is
to be employed. In using, on the other hand, the liquid
medium for the growth of cells through the culture with

2006260
~ ~ ~,..
the induced callus suspended, it is preferable to add
thereto 10 to 10 M of auxines, O to 10 5M, and l-lOwt.%
(with the basic liquid medium made as a reference) of
sugar. It may be possible to employ only either one of
auxines and cytokinins, in which event auxines should
preferably be employed. Further, copper ions detailed
later may also be added by O-20ppm as converted to copper
sulfate.
At the liquid medium to which callus is transplanted
after the foregoing suspension culture, the production of
the deodorizing ingredients is mainly carried out while
the tissue culture may also be carried out, and at least
one of cytokinins and copper ions is added here. Because
the added amount thereof is determinative to the effective
production of the deodorizing ingredients, it is
preferable that cytokinins will be about 10 7 to 10 3M,
and that copper ions will be about 5-lOOppm as converted
to copper sulfate, the copper ions being obtainable by an
addition of such salt as copper chloride, copper nitrate,
copper acetate, copper sulfate and the like. When the
added amount of salt is less than 5ppm, no sufficient
effect of providing the copper ions is attainable, while
the amount over lOOppm may cause a risk to arise in
hindering the cell from growing.
In extracting the ingredients effective as the
deodorant after completion of the culture, it may be
sufficient, for example, to filtrate the cells out of the
medium and, after a sufficient rinsing, to subject them to
-- 10 --

Z006260
an extraction for 0.5 to 5 hours at 20 to 90~C with water
or a mixture solvent of water and alcohol at a ratio of
1:9 to 1:1.
Examples of the present invention shall now be
described in the followings, along with comparative
example.
EXAMPLES 1-4
Organs of Forsythia koreana Nakai were cut into pieces
of 2-3cm, the cut pieces were sterilized by an aqueous
solution of ethanol, external plant sections of 1-2cm were
cut out of the organs under sterilized condition, and they
were bedded on the LS solid medium for inducing callus.
The LS solid medium used here consisted of 10 5M of
naphthalene-acetic acid, 10 7M of Kinetin, 10wt.% of sugar
and 0.7wt.% of agar (respectively with the basic liquid
medium made as a reference). The plant sections bedded on
such solid medium was cultured for 2 weeks at normal
temperatures to have callus induced.
Cells in logarithmic growth phase of Forsythia koreana
Nakai being cultured in the LS medium (with 3wt.% sugar
and 10 6M naphthalene-acetic acid added) after the callus
induction were transplanted to the White's medium (with
3wt.% sugar added, and pH being 5.6) to which each of such
different cytokinins as shown in Table I was added, and
the liquid culture was carried out among two weeks. After
this culture (cell concentration about 10wt.%), the cells
obtained were subjected to the filtration, rinse and
thereafter the hot water extraction for 4 hours at 50~C.
-- 11 --

2006260
An extract was diluted to be of 0.1wt.% concentration with
a buffer solution of pH 6.5 (of phosphoric acid), and
sample deodorants were obtained.
EXAMPLES 5-7:
Except for an addition of copper sulfate instead of
cytokinins, further sample deodorants were obtained in the
same manner as in the above EXAMPLE 1.
COMPARATIVE EXAMPLE 1:
A comparative sample deodorant was obtained from an
extract obtained from Forsythia koreana Nakai collected in
the month of October, in the same manner as in the above
EXAMPLE 1.
COMPARATIVE EXAMPLE 2:
A further comparative deodorant was obtained in the
same manner as in the foregoing EXAMPLES 1-7, except for
that no such additive as cytokinin and copper sulphate was
used.
A deodorizing test was carried out for the respective
deodorants obtained through the EXAMPLES 1-7 and
COMPARATIVE EXAMPLES 1 and 2, by means of a
gas-chromatograph equipped with a frame photometric
detector (FPD-GC). In carrying out the test, 2ml of the
deodorant in liquid phase was sealed within a container of
about 10ml, lml of methyl mercaptane gas
dilution-regulated was added by a gas bomb as an odorous
gas, they were stirred for 45 minutes, thereafter methyl
mercaptane concentration in head space gas was measured,
the deodorization rate with respect to water used for a
- 12 -

2006260
. .~
blank test (the deodorization rate with water being 0wt.%)
was calculated, and results were as listed in Table I as
follows:
TA ~ I
EX. Type of Additive Added Amount Deodorizing Rate(%)
1 N'-benzoyl adenine 10 M 95
2 2-hydroxypurin 10 3M 94
3 Benzyl adenine10 6M 93
4 Zeatin 10 5M 90
Copper sulfate5ppm 83
6 Copper sulfate20ppm 91
7 Copper sulfate100ppm 85
COMP .
EX.
1 (natural only) -- 90
2 (no additive) -- 80
It has been thus found that, as will be clear from the
above Table I, the deodorants obtained through the
respective Examples according to the present invention
show a deodorizing effect of the same level as or more
than that of the natural one according to COMPARATIVE
EXAMPLE 1, and that a remarkably improved deodorizing
effect can be attained as compared with COMPARATIVE
EXAMPLE 2 employing no such additive as cytokinin or
copper sulfate. It has been also found that, with copper
sulfate added less than 5ppm, the deodorant is less
effective and, even with its addition over 100ppm, the
effect is rather lowered.
- 13 -

2006260
~. .".
EXAMPLES 8-14:
Leafstalks of about lcm of such various Forsythia
genus plants as listed in Table II as follows were
subjected to a bactericidal treatment, bedded in an LS
solid medium (containing 3wt.% sugar, -6
naphthalene-acetic acid, 10 7M Kinetin, and lwt.% agar),
and the callus induction was carried out at 25~C. Callus
thus obtained in LS liquid medium with agar in the above
composition removed was suspended, 75ml of such suspension
was added in a flask (Meyer) of 300ml, and the culture and
growth were carried out under Meyer's shaking condition of
100 rpm rotation and at 25~C. The cells from latter half
of the logarithmic growth phase to the stationary phase in
the growth curve were transplanted to the White's medium
(containing 3wt.% sugar) to which a variety of cytokinins
such as listed in the following Table II and copper
sulfate were added, and further culture was carried out.
For the extraction of the deodorizing ingredients from
thus cultured cells, these cells were first filtered out
of the medium, sufficiently rinsed with water, and
thereafter subjected to the hot water extraction for 4
hours at 50~C, and thus obtained extract was concentrated
to be solid. The solid extract was prepared into lwt.%
aqueous solution and made to be a deodorant.
COMPARATIVE EXAMPLES 3-8:
As shown in the following Table II, cytokinin and
copper sulfate were added as required, and various
comparative samples of the deodorants were obtained in the
- 14 -

20()6260
same manner as in the foregoing EXAMPLES 8-14.
In respect of each of the deodorants obtained through
the above EXAMPLES 8-14 and COMPARATIVE EXAMPLES 4-8, the
deodorizing rate was calculated with water made as the
blank, by placing 0.1ml of the deodorant and l.9ml of a
buffer solution of phosphoric acid (pH 6.7) in a test tube
of 10ml, adding thereto lml of an odorous gas obtained
with methyl mercaptane (CH3SH) and a standard hydrogen
sulfide gas (H2S), and measuring residual odorous gas
concentration within the test tube after elapsing of 45
minutes by the foregoing FPD-GC, and measured values were
as listed in the following Table II:
TABLE II
EX. Plant Used Cytokinin Copper Deod. Rate(%,
Add. sUlfate CH SH H S
Used (M) (ppm) 3 2
8 Forsythia viridissima Kinetin 10 5 91 68
Lindl
9 Forsythia suspensa Benzyl adenine 10 30 90 73
Forsythia koreana Nakai 2-Hydroxypurin 10 90 93 72
11 Forsythia viridissima Phenyl aminopurin 10 7 20 90 69
Lindl
12 Forsythia suspensa 6-Methylpurin 10 100 83 69
13 Forsythia koreana Nakai N'-Benzoyl adenine 10 5 10 93 7114 Forsythia koreana Nakai Kinetin 10 6 70 92 75
COMP.
EX.
Forsythia koreana Nakai N'-Benzoyl adenine 10 6 __ 72 53
4 Forsythia suspensa --- --- 30 73 51
Forsythia suspensa Kinetin 10 -- 45 21

2006260
6 Forsythia koreana Nakai N'-Benzoyl adenine 10 150 (Brown death
of cells
7 Forsythia koreana Nakai Kinetin 5x10 -- 31 10
8 Forsythia viridissima --- --- -- 40 23
It has been found, as will be clear from Table II, that
the deodorants obtained through the EXAMPLES 8-14
according to the present invention have been provided with
further excellent deodorizing effect by the addition of
both of cytokinins and copper sulfate. As will be also
clear from the measured values for the deodorants of
COMPARATIVE EXAMPLES 3-8 in Table II, the deodorizing
effect is rather lowered when these additive members are
excessive over a proper range.
According to another feature of the present invention,
the deodorizing effect of the deodorant can be further
elevated by an addition of glyoxal to the deodorizing
ingredients extracted. While the amount by which glyoxal
is added is not required to be specifically limited, it is
preferable that the adding amount is 0.1-500 parts by
weight/l part by weight with respect to the extract 1.
Examples of this feature shall be referred to hereinunder
along with Comparative Examples.
EXAMPLES 15 and 16:
The deodorizing ingredients were extracted from
Osmanthus Lour. Var. Auranlacus Makino and Forsythia
suspensa, respectively, in the same manner as in the
foregoing EXAMPLE 1, and liquid extracts obtained were
concentrated to exsiccation by means of a rotary
- 16 -

2006Z60
evaporator. The exsiccated extracts were regulated with a
phosphoric acid buffer (0.15M) of pH 4.5 to render the
concentration of the deodorizing ingredients to be 0.1
weightwt.%. To these extracts, 40wt.% aqueous solution of
glyoxal was added, the concentration of this solution was
regulated to be of predetermined concentrations of lwt.%
and 5wt.%, and two deodorants were obtained.
COMPARATIVE EXAMPLES 9 and 10:
The same extracts as in the above EXAMPLES 15 and 16
were prepared to be two deodorants without addition of
glyoxal.
The respective deodorants obtained through these
EXAMPLES 15 and 16 and COMPARATIVE EXAMPLES 9 and 10 were
subjected to an evaluation of the deodorizing effect in
such manner that each solution of the respective
deodorants was put in a gastight container by a fixed
amount, trimethylamine (CH3)3N gas and methyl mercaptane
CH3SH gas were led into the container, and then the
container was sealed. A mixture gas in head space of this
container was thereafter collected, and the concentration
of trimethylamine and methyl mercaptane was measured by
means of the gas-chromatography. For the detection, FID
and FPD were employed, respective odor concentration in
the case where water was used instead of the deodorant
solutions were measured, and odor removal rate was
obtained according to a formula
Odor Removal Rate (%)={(A-B)/A}x100
wherein A was odor concentration in the case where water

Z006260
was used, and B was odor concentration in the case where
the deodorant was employed. Thus obtained values were as
listed in Table III as follows:
TABLE III
Deod. Ing. Glyoxal Deodorizing Rate(%)
EX. Plant Concent.(wt.%) Concent.(wt.%) (CH3)3N CH3SH
.
15 Osmanthus fragrans 0.1 1.0 94 89
~rs.Var. ~a~l~ M~
16 Forsythia suspensa 0.1 5.0 95 93
CO~P .
EX.
9 Osmanthus fragrans 0.1 -- 67 71
~rs.Var.~nai~I~ M~
Forsythia suspensa 0.1 -- 60 77
As will be clear from the above Table III, it has been
found that the deodorizing effect could have been
remarkably increased by the addition of glyoxal to the
extracted components from the plants.
EXAMPLES 17 and 18:
Deodorizing ingredients were extracted respectively
from Osmanthus X. Fortuneiu Carr and Lilac substantially
in the same manner as in the foregoing EXAMPLE 1 except
that the extraction was carried out at 60~C for 3 hours,
and the extracts were concentrated to exsiccation. Thus
extracted ingredients were regulated by phosphoric acid
buffer (0.lM) of pH 6.5 so as to be of a concentration of
0.5wt.%. 40wt.% aqueous solution of glyoxal was added to
the regulated ingredients so that glyoxal concentration
would be 0.25wt.%, and two deodorants were obtained.
- 18 -

Z006Z60
COMPARATIVE EXAMPLES 11 and 12:
Two deodorants were obtained from the same extracts as
in the above EXAMPLES 17 and 18 but without adding thereto
any glyoxal.
COMPARATIVE EXAMPLE 13:
Phosphoric acid buffer only was employed as a
deodorant.
Evaluation of the deodorizing effect was carried out
in a following manner with respect to the respective
deodorants obtained through the above EXAMPLES 17 and 18
and COMPARATIVE EXAMPLES 11-13. That is, a fixed amount
of each solution of the respective deodorants was put in a
container, an ammonia solution and hydrogen sulfide
solution were added thereto, and the container was sealed.
Thus obtained test samples were subjected to human
discrimination of odor intensity by five panelists having
the same degree of the sense of smell, with six grades of
the evaluation giving point "0" to no smell, "1" to very
slight smell, "2" to slight smell, "3" to easily sensible,
"4" to strong smell, and "5" to very strong smell, results
of which evaluation were as shown in a following Table IV
in the average value of the five panelists.
TABLE IV
Average Odor
Intensity by EX~LECOMPARATIVE EXAMPLE
5 Panelists 17 18 11 12 13
Ammonia 0.8 1.21.2 1.8 4.2
Hydrogen Sulfide 0.8 1.4 1.0 1.4 4.4
-- 19 --

2006260
In view of the above Table IV, it has been found that
the deodorizing effect could be improved to a large extent
by the addition of glyoxal. As a result of the same test
carried out as in the foregoing EXAMPLES 15-18 with
respect to other odor elements than the above two, it has
been also found that excellent effect could be attained
for any one of them. It has been further found that the
addition of glyoxal caused no variation in color phase of
the deodorant solutions nor any precipitation even after
being left for a long time, and a sufficient stability for
a time elapsing could be obtained.
According to still another feature of the present
invention, there can be provided a deodorant which is
improved in the deodorizing effect by an addition to the
extracted deodorizing ingredients at least one organic
acid selected from a group consisting of L-tartaric acid,
maleic acid, succinic acid, malic acid, citric acid and
lactic acid or the like, and/or one inorganic acid
selected from a group consisting of phosphoric acid, boric
acid and carbonic acid or the like, together with glyoxal
and a surface active agent. In this case, the addition of
the organic acid strengthens the deodorizing power with
respect to nitrogenous odors. While not required to be
limited specifically, the amount in which the organic acid
is to be added should preferably be 0.1 to 250 parts by
weight (in total when a plurality of the organic acids are
employed) with respect to 1 part by weight of the
extracts. Further, the addition of glyoxal allows the
- 20 -

2006Z60
foregoing action as has been described with reference to
EXAMPLES 8-18 to be attained, and its optimum adding
amount should be, when represented in the part by weight,
0.1 to 500 parts by weight with respect to 1 part by
weight of the extracts. With the addition of the surface
active agent, further, the deodorant can be maintained to
be uniform and also can be provided with a preservative
effect. For the surface active agent, any of cation
surface active agent, and ampho-ion surface active agent,
and its type is not specifically limited. While its
amount of addition is also not required to be specifically
limited, the amount may be in a range of 0.1-10 parts by
weight with respect to 1 part by weight of the extracts,
and the agent should preferably be benzalkonium chloride,
cetyl pyridinium chloride, benzetonium chloride or the
like as the cation surface active agent, or alkyl
polyaminoglycine or the like the ampho-ion surface active
agent.
In order to further elevate the deodorizing effect of
the deodorant prepared, further, it is desirable to
regulate the deodorant to be of a pH in a range of 3 to 8
by means of, for example, an addition of an alkaline
solution such as sodium hydroxide, potassium hydroxide or
the like, a solution having a buffer action such as a
phosphoric acid buffer or the like.
EXAMPLES 19-26:
Deodorizing ingredients were extracted from such
plants as listed in Table V as follows in the same manner
- 21 -

;~006260
~,,
as in the foregoing EXAMPLE 1, thereby obtained liquid
extracts were concentrated for exsiccation by means of a
Lawry's evaporator or a freezing dryer, and solid extracts
were obtained. With such extracts, water, an organic
acid, glyoxal and cetyl pyridinium chloride as a surface
active agent were added and mixed, sodium hydroxide was
added to thus obtained aqueous solutions, pH of which
solutions was regulated to be such predetermined values as
shown in a following Table V. Ethanol was added at such
various amounts as shown in a following Table V to the
respective solutions pH-regulated, and sample deodorants
of EXAMPLES 19-26 were obtained.
In the following Table V, the amount of ethanol added
is presented in the part by weight with respect to 1 part
by weight of liquid state mixture of ethanol with the
plant extracts, organic acid, glyoxal and so on, pH of
which has been regulated.
COMPARATIVE EXAMPLE 14:
A sample deodorant was obtained substantially in the
same manner as in EXAMPLE 19 except for that lactic acid
was not added.
COMPARATIVE EXAMPLE 15:
A sample deodorant was obtained substantially in the
same manner as in EXAMPLE 19 except for that glyoxal was
not added.
COMPARATIVE EXAMPLE 16:
A sample deodorant was obtained substantially in the
same manner as in EXAMPLE 19 except for that cetyl
- 22 -

2006260
pyridinium chloride as the surface active agent was not
added.
COMPARATIVE EXAMPLE 17:
A sample deodorant was obtained substantially in the
same manner as in EXAMPLE 19 except for that lactic acid,
glyoxal and cetyl pyridinium were not added at all.
- 23 -

Z006260
. .,,.,~
4~ ~ In
_ a ~ ~o~ ~ ~ ~ Oc~ ~ ~ ~ I
0 0\o
~ 00 0 ~0 ~ U' O O ~ ~
. . o O O O o o o o o o
q
- ~ ~ o~ In O O ~ O O ~D
C~ ~ o o o ~ ~ ~ ~ ~ o I O
~o ~
~ o o o o o o o o I O O
,~
.,,
~~ ~ C ~ C ~ I ~ C
~ 3 ~ q q q ~ q ~ q
~ o o o ~ o o o ~ ~ ~ ~
- ~
tJ o ~
u l - o r ~ ~o l ~ ~ ~ cl ~l c ~ o
rl ~ ,~ ¢~ I ~ ¢~ r- ''I ~ f '. r ~ r
O ~ ~ ~ O ~
X
-- 24 --

2006Z60
~e
The respective sample deodorants obtained through the
above EXAMPLES 19-26 and COMPARATIVE EXAMPLES 14-17 were
subjected to the deodorizing test after leaving them as
they stood for 24 hours. That is, a fixed amount of each
5 of the sample deodorants was put in a container as
atomized, ammonia gas, hydrogen sulfide gas or methyl
mercaptane gas was added thereto to a level providing a
very strong odor, and the container was sealed. The same
human discrimination of the intensity of odor with the six
10 grade evaluation of "0" to "5" as in the foregoing
EXAMPLES 17 and 18 and COMPARATIVE EXAMPLES 11-13 was
carried out by five panelists having the same level of the
sense of smell, results of which were as shown in Table VI
in the following, in average value:
TABLE VI
Average Odor
Intensity by Example Comp. Example
5 Panelists _ 20 21 22 23 24 25 26 14 15 16 17_ _ _ _ _ _ _ __
NH3 0.8 0.4 1.2 0.8 1.0 0.4 0.2 0.8 1.8 0.8 1.0 2.0
H2S 0.8 1.2
CH3SH 0.8 - 0.4 0.0 0.4 1.2 1.0 0.8 0.8 1.6 1.0 1.8
It has been found as would be clear from the above
Table VI that, according to the present feature, the
offensive odor of nitrogen series and sulfur series could
be deodorized to the level of no smell or at least very
slight smell, whereas the deodorants of the Comparative
Examples were much deteriorated in the deodorizing power
-- 25 --

Z006260
as compared with those of the present feature. That is,
it will be appreciated that the deodorant of COMPARATIVE
EXAMPLE 14 having no organic acid is lower in the power of
deodorizing the nitrogen series odor, the one of
COMPARATIVE EXAMPLES 15 with no glyoxal added is low in
the power of deodorizing the sulfur series odor, the one
of COMPARATIVE EXAMPLE 16 with no surface active agent
added is low in the deodorizing power for both of the
nitrogen and sulfur series odors, and the one of
COMPARATIVE EXAMPLE 17 is considerably low in the
deodorizing power for both of the nitrogen and sulfur
series odors. The same panelists' test as in the above
has been also carried out with respect to such other odors
than the above as trimethyl amine, nicotine and lactic
acid, excellent results could be attained with the
deodorants of the present feature. In addition, a state
observation of the deodorants according to the present
feature has shown results excellent in the stability for
the time elapsing, without involving any variation in
color phase nor precipitation.
Aspects in which the deodorants according to the
present invention as has been described are utilizable can
be selected over such a wide range as a liquid agent,
spraying agent, impregnation in a proper carrier, powdery
agent, tablets, granular agent and so on, depending on the
use and environment in use. When the deodorant is used as
the spraying liquid sealed in cans (with any known canning
method employed), and as the impregnation in a filtering
- 26 -

2006260
..--
member or stick, its possibility of general use is more
improved.
In using the deodorant according to the present
invention in the aspect of the spraying agent, the
deodorant obtained through the process as has been
described can be utilized as it is, while any proper
additive or additives may be added for the purpose of
improving deodorizing effect or preservability in the
canned state of the agent. In this case, a preferable
composition will be of the deodorant, organic and/or
inorganic acid, glyoxal and the surface active agent, pH
of which should desirably be adjusted to be in a range of
pH 3-8 with any agent admixed as has been described. In
preparing the spraying agent, further, it is preferable to
add ethanol to the deodorant composition at 0.1 to 99
times by weight of total weight of the composition of
other components than ethanol.
- 27 -

Representative Drawing

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Administrative Status

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Event History

Description Date
Time Limit for Reversal Expired 2004-12-20
Letter Sent 2003-12-22
Grant by Issuance 1999-03-16
Pre-grant 1998-11-25
Inactive: Final fee received 1998-11-25
Notice of Allowance is Issued 1998-05-26
Letter Sent 1998-05-26
Notice of Allowance is Issued 1998-05-26
Inactive: Status info is complete as of Log entry date 1998-05-21
Inactive: Application prosecuted on TS as of Log entry date 1998-05-21
Inactive: IPC assigned 1998-04-09
Inactive: IPC removed 1998-04-09
Inactive: First IPC assigned 1998-04-09
Inactive: Approved for allowance (AFA) 1998-04-03
Application Published (Open to Public Inspection) 1991-06-20
All Requirements for Examination Determined Compliant 1989-12-20
Request for Examination Requirements Determined Compliant 1989-12-20

Abandonment History

There is no abandonment history.

Maintenance Fee

The last payment was received on 1998-12-14

Note : If the full payment has not been received on or before the date indicated, a further fee may be required which may be one of the following

  • the reinstatement fee;
  • the late payment fee; or
  • additional fee to reverse deemed expiry.

Patent fees are adjusted on the 1st of January every year. The amounts above are the current amounts if received by December 31 of the current year.
Please refer to the CIPO Patent Fees web page to see all current fee amounts.

Fee History

Fee Type Anniversary Year Due Date Paid Date
MF (application, 8th anniv.) - standard 08 1997-12-22 1997-11-19
Final fee - standard 1998-11-25
MF (application, 9th anniv.) - standard 09 1998-12-21 1998-12-14
MF (patent, 10th anniv.) - standard 1999-12-20 1999-11-05
MF (patent, 11th anniv.) - standard 2000-12-20 2000-11-17
MF (patent, 12th anniv.) - standard 2001-12-20 2001-11-19
MF (patent, 13th anniv.) - standard 2002-12-20 2002-11-19
Owners on Record

Note: Records showing the ownership history in alphabetical order.

Current Owners on Record
MATSUSHITA ELECTRIC WORKS, LTD.
Past Owners on Record
HARUYUKI DATE
MANABU MIZOBUCHI
TOSHIYUKI YAMAUCHI
YASUHIRO SAIHARA
Past Owners that do not appear in the "Owners on Record" listing will appear in other documentation within the application.
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Document
Description 
Date
(yyyy-mm-dd) 
Number of pages   Size of Image (KB) 
Abstract 1994-04-17 1 9
Description 1994-04-17 26 773
Claims 1994-04-17 5 154
Description 1998-03-17 26 865
Claims 1998-03-17 4 177
Commissioner's Notice - Application Found Allowable 1998-05-25 1 164
Maintenance Fee Notice 2004-02-15 1 175
Correspondence 1998-11-24 1 37
Fees 1996-10-20 1 44
Fees 1995-10-19 1 42
Fees 1994-11-03 1 38
Fees 1992-12-07 1 35
Fees 1993-11-15 1 34
Fees 1991-10-28 1 34
Courtesy - Office Letter 1990-06-13 1 19
Prosecution correspondence 1993-12-29 2 46
Prosecution correspondence 1993-04-22 2 41
Examiner Requisition 1992-10-29 1 72
Examiner Requisition 1993-08-31 2 61