Note: Descriptions are shown in the official language in which they were submitted.
2~~~~~~
WO 92/11002 PCT/iJS91/09337
1
wF°r POtrdDFR FII~-POR1~I1NG Cp~LpOSTT'~OPIS
This application is a continuation-in-part of
application Serial No. 630.815, filed December 20, 1990.
This invention relates to film-forming or film
coating compositions for use in the film coating of
pharmaceutical tablets and the like and, more particularly,
to such compositions in the form of wet powder blends or wet
powder, clear, film-forming compositions.
Signorino U.S. patent no. 3,981,984 discloses
edible concentrated pigment suspension in which pigments are
suspended in non-aqueous solvents. Such pigment suspensions
are shipped, for example, to pharmaceutical manufacturers who
mix them With polymer solutions to form coating suspensions
used for coating tablets and the like. Each of the pigment w
suspensions, polymer solutions and coating suspensions formed
therefrom are in a non-aqueous solvent.
Porter et al. U.S. patent no. 4,593,370 discloses a
dry edible film coating composition for use in
pharmaceuticals, confectionary and food which comprises a
mixture including pigment particles, polymer particles, a
polymer plasticizer such as polyethylene glycol 400 and,
advantageously. a surfactant such as dioctyl sodium
sulfosuccinate. According to the patentees, such a film
coating composition responds to a long standing desire to
provide a dry edible film coating composition which can be
constituted with solvent by the customer, that eliminates the
problem of shipping of pigment dispersions containing aqueous
or non-aqueous solvents, and also makes shipping less
expensive by eliminating. the weight o~ the solvents. In U.S.
patent no. 4,543,370 it is stated to be known in the prior
WO 92/11002 ~ ~ '~ P(.T/U~9110933.
2
art to mix a dry polymer powder with pigment particles arid to
grind the mixture to obtain a dry polymer-pigment mixture
which is then ground into a fine powder mixture. However, as
further stated in this patent, when this fine polymer-pigment
mixture is stirred into water and dispersed, the polymer
makes lumps and fish eyes because it agglomerates and the
resultant dispersion is not uniform. When this polymer-
pigment dispersion is used as a coating dispersion and is
coated onto tablets and the like, unless the
dispersion is left to solvate for a considerable period of
' time like overnight, the coating is lumpy and not uniform.
The dry coating compositions of U.S. patent no.
4,543,370 are stated to be useful within an hour of being
made up and not to require an overnight waiting period as was
required by prior art aqueous and non-aqueous systems.
Heinze U.S. patent no. 4,636.261 discloses dry
mixtures of powdered edible pigment particles and a
dispersing agent which prevents agglomeration and facilitates
dispersion into solution. The dispersing agent may be the
salt of an organic compound containing one to four carboxylic
acid groups or a salt of phosphoric acid.
In the preparation of clear film coating
compositions for coating aspirin tablets and the like, it has
heretofore been the practice to dissolve or disperse a
polymer such as hydroxypropylmethyl cellulose in water and
then wait for a period of 1~ hours or so before applying the
resulting polymer solution or dispersion to tablets or the
. like. Such a waiting period has been deemed necessary in
order to rid the solution or dispersion of fish eyes and
allow water to penetrate into or hydrate the polymer gel
particles (fish eyes) which form upon dissolving or
dispersing the polymer in water. While pre-conditioned or
surface-treated polymers are available, it is necessary to
add a base material to such polymers in order to allow the
~~~~~J~
WO 92/11002 . PCf/US91/09337
3
polymers to become hydrated and dissolve or disperse in water.
There remains a need for further improvements in
film coating compositions with regard to their ability to
disperse color in the coating of tablets, capsules and the
like and their usefulness for this purpose upon pregaration
or within a short time thereafter.
Summary c,Zf the Invention
Among the objects of the present invention may be
noted the provision of film-forming compositions useful in
coating tablets, capsules and the like which are produced in ""
the form of wet powder blends; the provision of clear
film-forming compositions for use in coating tablets and
capsules with a clear coating; the provision of such
compositions which are capable of forming stable suspensions
for coating tablets, capsules or the like upon dilution with
additional water; the provision of compositions of this type
which can be used for coating tablets and capsules shortly
after being combined with additional water and a plasticizer;
and the provision of methods of making such film--forming
compositions. Other objects and features will be in part
apparent and in part pointed out hereinafter.
Briefly, the present invention is directed to a wet
powder, edible, film-forming composition for use i~n coating
tablets, capsules and the like which consists essentially of
powdered pigment particles, a film-forming, water-soluble or
water-dispersible, edible polymer and between approximately
1% and approximately 30% by weight of water, the composition
being formed by blending the pigment particles and polymer
and applying the water onto the pigment-polymer blend in
atomized form and the composition being capable of forming a
stable suspension upon dilution with additional water.
Preferably, the composition also contains a dispersing agent
..
WO 92/11002 PCT/US91/0935
4
such as an alkali metal or ammonium salt of ethylene diamine
tetraacetic acid which lowers the surface tension of water in
the composition.
The invention is also directed to a method of
making a wet powder, edible, film-forming composition of the
type described above for use in coating tablets, capsules
and the like which comprises (a) blending powdered pigment
particles and a film-forming, water-soluble or
water-dispersible edible polymer; and (b) applying water or
an aqueous solution of the above--mentioned dispersing agent
onto the pigment-polymer blend in atomized form, the
composition containing between approximately 1°s and
approximately 30°s by weight of water.
The invention, in another embodiment, is further
directed to a wet powder, edible, clear, film-forming
composition for use in coating tablets, capsules and the like
with a clear coating consisting essentially of a clear, ,'
film-forming, water-soluble or water-dispersible, edible
polymer and between approximately 1% and approximately 30°a by
weight of water, the compositions being formed by applying
water onto the polymer in atomized form and the composition
being capable of forming a stable suspension upon dilution
with additional water without the formation of fish eyes.
The composition of this emobidment of the~invention
preferably also contains a dispersing agent of the
aforementioned type, and the invention further encompasses a
method of making a clear, film-forming composition of this
embodiment.
pescr'.~~:LC~n of the pre~er~ec~ ld~x~ts
In accordance with the present invention, it has
now been unexpectedly found that useful wet powder, edible,
film-forming compositions for coating tablets, capsules and
2~9~~3~~
dV0 92/11002 . PGT/US91/09337
the like may be formulated by blending powdered pigment
particles with a film-forming, water-soluble or
water-dispersible, edible polymer and applying water onto the
pigment-polymer blend in atomized~form. When formulated in
5 this manner, the resulting film--forming' compositions have
been found capable of tolerating up to approximately 30% by
weight water while yet remaining capable of forming a stable
suspension upon dilution with additional water. Also, the
film-forming compositions prepared in accordance with the
present invention and containing between approximately 1% and
approximately 30% by weight of water do not lump up or
contain fish eyes and, when combined with additional water
and a plasticizer provide a smooth, uniform coating for
pharmaceutical tablets, capsules and the like. Optionally,
but preferably, the film-forming compositions of the
invention also contain a dispersing agent constituted by an
acid salt which lowers the surface tension of the water in
the composition and which in turn lowers the viscosity of the
final coating suspension to thereby provide improved and
smoother coatings for tablets and the like.
It is believed that the addition or application of
water onto the pigment-polymer blend in atomized form in
accordance with the invention advantageously preconditions
the polymer and avoids clumping or the formation of fish eyes
when~,the compositions of the invention are added to water to
form coating suspensions. Thus, by applying the water, in
atomized form, the water becomes uniformly distributed over
or to all polymer particles, the pigment particles adhere to
the polymer particles and the polymer is preconditioned so
that hydration of the polymer is expedited when the
pigment-polymer blend is dispersed in water to form a coating
suspension. Accordingly, the present invention achieves the
advantageous preconditioning of the blend of pigment and '
polymer causing the blend to readily disperse and dissolve in
a
CA 02098834 2002-12-31
72037-17
6
water in forming the desired coating suspension without
deleterious lumping or agglomeration. Moreover, through the.
. present invention, it becomes possible to prepare smooth w
coating suspensions which can be used immediately or Within
w
30 minutes for the coating of tablets or the like,
In the practice of the present invention, powdered
pigment particles are first blended or admixed with a
film-forming, water-soluble or water-dispersible, edible '
polymer. Water or an aqueous solution of a dispersing agent'
which lowers thesurface tension of water is then applied
onto the pigment-polymer blend in atomized form to produce
a'
film-forming composition containing between appro8imately 1%'
and approximately 30$ by weight of water. For use as the'.._
~~ .
~
powdered pigment component of the compositions of the
' ~ -
invention, any FDA approved edible natural or synthetic .
colorant may be employed. Useful. pigments include, but are'
.
not limited ta, FD&C and D&C dyes, FD&C and D&C lakes, ,
titanium dioxide, iron oxides, talc, alumina, silica and
natural colorants. Typically, the powdered pigment particles
may be constituted by a combination of a lake and titanium
~
dioxide or iron a~aide. The particle size of the powdered .
pigment particles is not critical, but the finer the particle
size, the better the results achieved through the present
invention. The particle size of commercially available
pigments known to those in the art renders them satisfactory
~..
for use in the compositions of the invention. ~.
In order to be useful in the invention, the
film-forming, edible polymer component must be water-soluble
or water-dispersible. Useful polymers of,this type include
methyl cellulose, hydro~cypropylmethyl cellulose, .
hydroaypropyl cellulose, polyvinyl pyrralidone, maltodeatrin,
polydextrose, modified starches {such as "Purity Gum 59".,
~
gum.
marketed by National Starch) and natural gums such as
tragacanth, gum acacia and xanthan-gums, with _
CA 02098834 2002-12-31 '
72037-17
7
hydroxypropylmethyl cellulose being the preferred polymer.
Mixtures of such polymers may also be used. It is preferred
that the polymer be in powdered form, but the particular
particle size of the polymer is not critical. in the practice
of the invention.
After the powdered. pigment and polymer. have been
blended until uniform, the desired amount of water per se or
in the form of an aqueous solution of a dispersing agent is
added with intense miaing.so that the water or aqueous
solution of the dispersing agent is applied to the pigment-
polymer blend in atomized form. This can be accomplished,
for example, by blending.the powdered pigment and polymer in
a PK Blender~"or a Littleford~'FM 130 Blender and adding the
water or aqueous solution of dispersing agent with intense
mixing by fine atomization into the blender chamber where the
powdered pigment and golymer are being mixed. Preferably,
the water or aqueous solution is added slowly and the
resulting water-containing blend or composition is mixed
intensely after addition of the water.
It has been found that film-forming compositions
prepared in this manner may contain up to approximately 30%
by weight of water and yet remain capable of forming a stable
suspension useful for coating tablets and the like upon'
dilution with additional water. It should be noted that
where FD&C lakes are employed as pigments, they may contain
up to IS~C by weight of .water and that the polymer component
may likewise contain up to 4% to 5% by Weight of water. The
water added through the practice of this invention is
additional water over and above that contained in the pigment
34 and polymer components and, as stated, may range from
approximately 1% to 30% by weight, with approximately 2% to
10% by weight being the preferred among and approximately 5%
to 9% by weight being the most preferred amount.
In an optional but highly preferred embodiment. a
ffO 92/11002 ~ o ~ ~ ~~L~. P(;lf/US91/0933,
a
dispersing agent which lowers the surface tension of water is
incorporated into the film-forming compositions of the
invention. The dispersing agent is constituted by an acid
salt which functions to lower the surface tension of water in
the compositions and illustrative acid salts which perform
this function include the alkali metal and ammonium salts of
ethylene diamine tetraacetic acid, nitrilo triaacetic acid,
citric acid, phosphoric acid, tartaric acid, glycolic acid, ,'
malic acid, lactic acid, acetic acid and benzoic acid. It
1G will be understood that other acid salts which function to
lower the surface tension of water in the compositions may
also be employed in the practice of the invention. Sodium
salts of ethylene diarnine tetraacetic acid represent the
preferred dispersing agents for use in the practice of the
invention. The dispersing agent is generally: incorporated
into the film-forming compositians in the form of aqueous
solutions of such acid salts, such aqueous solutions being
applied to the pigment-polymer blends as previously described
and providing the amount of water to be added to the
compositions as well as acting as the vehicle for the
application of the dispersing agent to the pigment-polymer
blends. Alternatively, but less preferably, the dispersing
agent may be added in powder form to the pigment-polymer
blend~with the water being applied to the resulting blend of
the three components in atomized form. The dispersing agent
not only lowers the surface tension of the water in the
film-forming compositions of the invention but also lowers
the viscosity of the coating suspensions prepared from such
compositions thereby providing smaller suspension droplets
and smoother coatings for tablets and the li~,e. While the
invention may be practiced without the addition of a
dispersing agent to the film-forming compositions, it has
been found that the incorporation of a dispersing agent
produces a better color development and quality of coating
WO 92/11002 . PCT/US911093~7
9
for tablets and the like.
The film-forming compositions. of the invention are
shelf-stable for extended periods of time without the use of
preservatives and are not prone to settling or other
break-downs. Further, it is believed that such compositions
remain free from bacteria formation such as may be normally
caused by the solvent in liquid pigment dispersions.
To prepare coating suspensions for use in coating
tablets and the like, the film-forming compositions of the
invention are added to water and~a plasticizer in accordance
with conventional practice. The coating suspensions so
grepared may be applied immediately to tablets without a
waiting period such as overnight as is required with certain
prior art systems. Any of the plasticizers known to the art
such as polyethylene glycol 400, glycerin, propylene glycol,
glycerine triacetate, triethyl citrate, tributyl citrate or
diethyl phthalate may be used in formulating coating
suspensions from the wet film-forming compositions of the
invention.
In another, but lass preferred, embodiment of the
invention, a plasticizer may be incorporated into the wet
film-forming compositions of the invention so that the
resulting compositions may be simply added to water in order
to form useful coating suspensions for coating tablets and
the like. '
In preparing the wet powder, edible, film-forming
compositions of the invention, the proportions of pigment and
polymer employed are not critical. In general, where the
ratio of pigment to polymer is high, a flat appearing film of
lower quality will be obtained whereas with lower ratios of
pigment to polymer, a more glossy film finish and better film
properties will be obtained. For acceptable results, the
weight ratio of polymer to pigment should range between 1.5:1
and 3:1 with the ratio of approximately 2.5:1 being
~Cf/~~J~v: i
dV0 92111002
preferred where the pigment component is primarily
constituted by a lake. ,
The proportion of dispersing agent incorporated
into the film-forming compositions of the invention may vary
S widely but, in general, may constitute between 0.1 to 5.0% by
weight based on the weight of the pigment and polymer
components and more preferably between 0.5 to 2.0% by weight.
In another embodiment and in further accordance
with the invention, it has also been unexpectedly found that
10 useful wet powder, edible, clear film-forming compositions
for coating tablets, capsules and the like with a clear
coating may be formulated by applying water onto a
film-forming, water-soluble or water-dispersible, edible,
clear polymer in atomized form. F~ere again, when. formulated
in this manner, the resulting clear, film-forming
compositions have been found capable of tolerating up to
approximately 30% by weight water without forming fish eyes
while yet remaining capable of forming a stable suspension
upon dilution with additional water. such clear, film-
ZO forming compositions prepared as described above and
containing between agproximately 1% and 30% by weight of
water do not lump up or contain fish eyes and therefore
require no long waiting period or pretreatment of the polymer
component before being used to make coating compositions.
When combined with additional water and a plasticizes, such
clear, film-forming compositions yield a smooth, uniform
coating composition for coating pharmaceutical tablets,
capsules and the like With a clear coating. When a
plasticizes is incorporated,.water is first applied onto the
polymer in atomized form following which the plasticizes is
sprayed onto the resulting composition. Through this
embodiment of the invention, it becomes possible to prepare
smooth, clear, coating suspensions which can be used
immediately or within 30 minutes for providing tablets,
~~~~U~~
WO 92/11002 P(:T/US9a/09337
11 ,
H
capsules- or the like with a clear coating. In this
embodiment of the invention, it is also optional, but
preferable, for the clear, film-forming compositions to
contain a dispersing agent constituted by an acid salt which
lowers the surface tension of the water in the composition.
Any of the dispersing agents enumerated above may be used in
this embodiment of the invention.
In forming clear, film-forming compositions as
above described, it is believed that the application of water
onto the polymer advantageously preconditions the polymer as
in the case of the pigment-polymer blend described above and
avoids clumping or the formation of fish eyes either upon
application of the water or when the resulting clear,
film-forming compositions of the invention are added to water
to form coating suspensions. Upon the application of water
to a clear polymer as previously described, granules or an
agglomeration of polymer particles are formed which
unexpectedly go into solution readily in contrast to the
addition of a polymer per se to water which tends to clump or
form fish eyes. In forming clear, film-forming compositions
of the invention in accordance with this additional
embodiment, the same film-forming, water-soluble or
water-dispersible, edible polymers, dispersing agents and
plasticizers disclosed above may be employed, but the
resulting compositions are.clear because they contain no
pigment component. Also, such clear, film-forming
compositions can be prepared using a PK Blender or a
Littleford FM 130 Hlender which insure that the water is
applied to the polymer in atomized form. The water may also
be applied in atomized form by means of an aqueous solution
of the dispersing agent where the latter is optionally but
preferably incorporated into the film-forming compositions.
The following examples illustrate the practice of
the invention.
Vf~ 92/11002 PCT/US91/0933
12
Example 1
The following ingredients were charged to a
Littleford FM 130 blender:
Hydroxypropylmethyl cellulose 93 lb.
Titanium dioxide 26 lb.
FD&C Yellow 6 Low dye lake 1 lb.
The ingredients were blended for two minutes to form a
pigment-polymer blend. 3.5 lb. of a 10°s aqueous sodium
citrate solution was sprayed onto the pigment-polymer blend
1~ s~rith mixing in approximately 2.5 minutes and then mined for 1
minute after addition of the sodium citrate solution was
complete. This effected application of the sodium citrate
solution onto the pigment-polymer blend in atomized form. A
dustless, free-flowing powdered film-forming composition was
produced.
example 2
The following ingredients weze charged to a
Littleford W-10 mixer:
Hydroxypropylmethyl cellulose 1.36 kg.
Titanium dioxide 0.35 kg.
FD&C Yellow 5' High dye lake 0.20 kg.
FD&C Yellow 6 High dye lake 0.03 kg.
The ingredients were mixed for three minutes to form a
pigment-polymer blend. 60 grams of a 10% aqueous solution of
the tetrasodium salt of ethylene diamine tetraacetic acid was
then sprayed onto the pigment-polymer blend in one minute,
with mining continued for one minute after the addition of
the 10% solution Was complete. A dustless, free-flowing
powder was produced.
Example 3
The following ingredients were charged to a PK
Blender Model LBC-2P:
Hydroxypropylmethyl cellulose 900 g.
Titanium dioxide 100 g.
;:, . . . . . - ;, . , < ~, ;,;, :, ,~ _ J,;,,.. , .;:. .
PC'T/US91/0~3~7
W0 92/11002
13
FD&C Yellow 6 High dye lake 100 g.
The ingredients were mixed for four minutes to form a
pigment-polymer blend. 60 grams of water was then sprayed
onto the pigment-polymer blend in two minutes, with mixing
continued for one minute after the addition of the water was
complete. A ductless, free-flowing.powder was produced.
l~a~am~le 4
Example 3 was repeated using 60 grams of a l00
aqueous solution of the tetrasodium salt of ethylene diamine
tetraacetic acid in place of water. A ductless, free-flowing
powder was produced.
E~am~'L~ S
Example 3 was repeated using 60 grams of a 10%
aqueous solution of sodium citrate in place of water. A
15. ductless, free-flowing powder~was produced.
EaamP ~P~6.
Example 3 was repeated using 30 grams of a 10%
aqueous solution of sodium dibasic phosphate (Na2HP04)in
place of water. A ductless, free-flowing powder was produced.
2 0 am~~
Example 3 was repeated using FD&C Red 40 in place
of FD&C Yellow 6 High dye lake. A ductless, free-flowing
powder was produced.
Example 8
25 Example 3 was repeated using FD&C Red 40 in place
of FD&C Yellow 6 High dye lake and 30 grams of a 10% aqueous
solution of the trisodium salt of ethylene diamine
tetraacetic acid in place of water. A ductless, free-flowing
powder was produced.
30 F~~ample 9
A coating suspension was prepared as follows: 87.5
grams of water and 1.'S grams of polyethylene glycol 400 were
charged to a beaker. While stirring the beaker contents
vigorously; 11 grams of the powder produced in Example 4 was
WO 92/11002 ~ ~ ~ ~ ~; '~ ,'3 PGT/U591/09~'~
lJ cJ .i
14
added to the beaker. The powder readily dispersed and the
suspension which formed thickened and became very smooth in
15 minutes.
The resulting co~a,ting suspension was applied
inunediately to tablets in a 4" wurster Column, and a smooth
glossy coating on the tablets was achieved in 15 minutes.
Ql.e ~0
The following ingredients were charged to a PK
Blender Model LBC-2P:
Hydroxypropylmethyl cellulose 360 g.
Maltrin M-100 (Maltodextrinj 240 g.
The above polymer ingredients should preferably be
distributed equally in each shell of the blender and should
be 1/2 to 3/4 the way up the intensifier bar of the blender.
The blender was closed and mixing of the dry blend was
carried out for 4 to 5 minutes with both the shell and
intensifier bar mixing being used. After the polymer
ingredients were thus blended, mixing with both the shell and
intensifier bar was continued and the liquid feed pump was
turned on. 38 grams of a 10% aqueous solution of sodium
citrate was fed onto the polymer blend in atomized form
followed by the addition of 48 grams of polyethylene glycol
400 as a plasticizer. After the addition of the sodium
citrate solution and plasticizer, the liquid feed pump was
allowed to run for 1 minute to clear the lines. After the
liquid feed pump was shut off, the shell and intensifier bar
were allowed to mix for 30 seconds and the blender was shut
' off. A ductless, free-flowing powder was produced.
~amp~, a 11
The composition of Example 10 was used to make a
coating solution. 863.2 grams of water were added to a
container equipped with a variable speed mixer. The mixer
was started and once a vortex was formed, 136.8 grams of the
composition of Example 10 was added in a steady and
dV0 92/11002 ~ ~ ~ ~ ~ J ~ PCT/US91/09337
consistent manner. The speed of the mixer was increased as
the solution became more viscous, with the composition being
added to the center of the vortex for best mixing. After the
complete addition of the Example 10 composition, the speed of
5 the mixer was reduced to reduce aeration of the solution.
The sides of the container were scraped to remove any clumps
which were added to the center of the solution. Mixing was
continued for 30 minutes to produce a smooth, clear coating
solution.
The clear, coating solution of Example 11 was used
to coat tablets by column or pan coating. The coating
solution of Example 11 was charged to the liquid feed system
and the tablets to be coated were charged to the coating
equipment. The tablets were warmed and the coating solution
was sprayed onto the tablets. The resulting tablets had a
smooth, clear, glossy coating.
mo ~ 13
The procedure of Example 10 was generally followed
20. to produce a wet powder, edible, clear, film-forming
camposition having the following composition:
~r,~ponent Wt-
Hydro$ypropylmethyl cellulose 68.2
Hydroxypropyl cellulose 22.8
Water . 9.0
A dustless, free-flowing powder was produced.
a mp 1~ 14
The procedure of Eaample 10 was generally followed
to produce a wet powder, edible, clear, film-forming
composition having the following composition:
~ompoLL~.n~.
Hydroxypropylmethyl cellulose 94.6
Sodium citrate 0.4
Water 5.0
A dustless, free-flowing powder was produced. .
WO 92/11002 ~ ~ ~ ~ ~ ~ ,~ PCf/iJ~°~ ° % r"'' ;
16
Example 15
The procedure of Example 10 was generally followed
to produce a wet pocvder, edible, clear, film-forming
composition having the following composition:
Co~~onent ~ wt . %.
Hydroxyprogylmethyl cellulose 91.5
Sodium citrate 0.4
Water 8.1
A dustless, free-flowing powder was produced.
E xam~~,e~
The procedure of Example ZO was generally followed
to produce a wet powder, edible, clear, film-forming
composition having the following composition:
Component W~. °.
Hydroxypropylmethyl
cellulose ~ 84.0
Sodium citrate 1.0
Talc 5.0
Glycerin triacetate 5.0
Water 5.0
A dustless, free-flowing powder was produced.
Exammle 17
The procedure of Example 10 was generally fol~locaed
to produce a wet powder, edible, clear, film-forming
composition having the following composition:
Component _ Wt-
Hydroxypropylmethyl cellulose 87.70
Sodium citrate 0.14 .
Talc 3.90
Glycerin triacetate 4.30
Water 3.90
A dustless, free-flowing powder was produced.
Example 18
The procedure of Example 10 was generally followed
to produce a wet powder, edit~le, clear, film-forming
WO 92/11002 ~ ~ ~ ~ ~ ~ ~ ~ h~y.'.I,::,-; ;~~::- ::'7
17
composition having the following composition:
Component Wt~.
Hydroxypropylmethyl cellulose 90.3
Tetrasodium ethylene diamine
,
tetraacetate 0.5
Polyethylene glycol 4.5
water 9.7
A dustless, free-flowing powder was produced.
F~ramgle 19
The procedure of Example 10 was gen erally followed
to produce a wet powder, edible, clear, f ilm-forming
composition having the following composition:
f:omponent Wt . %.
Hydroxypropylmethyl cellulose 85.4
Tetrasodium ethylene diamine
tetraacetate 05
Polyethylene glycol 43
water 4.6
A dustless, free-flowing powder was produced.
E~amnle 20
The procedure of Example 10 was generally
followed
to produce a wet powder, edible, clear, film-forming
composition having the following composition:
n
Component wt . ~s
Hydroaypropylmethyl cellulose 91.5
Triethyl citrate 46
Water 3.8
A dustless, free-flowing powder was produced.
21
l
examp nerally followed
e
The procedure of Example ZO was ge
to produce a wet powder, edible, clear, film-forming
composition having the following composition:
omgon n
Hydroxypropylmethyl cellulose 84.50
WO 92/11002 z a ~ ~ ~ a. ::~ ~~~~.~E..~, : ,.,.,., ,.
18
Sodium citrate 0.35
Glycerine triacetate 8.50
Talc 3.50
Water 3.20
A dustless, free-flowing powder was produced.
2
~~am~.~e a rally followed
The procedure of Example 10 was gene
to produce a wet powder, edible, clear, f ilm-forming
composition having the following composition:
Component wt.~
Hydroxypropylmethyl cellulose 84.50
Sodium citrate 0.35
Glycerin triacetate 8.00
Talc 4.00
Water 3.20
A dustless, free-flowing powder was produced.
23
exam a
The procedure of Example 10 was generally
followed
to produce a wet powder, edible, clear, film-forming
composition having the following composition:
CrOmDOnent
Hydro~cypropylmethyl cellulose 85.50
Sodium citrate 0.35
Glycerin triacetate 6.00
Talc 5.00
Water ,3.20
A dustless, free-flowing~powder was produced.
24
l
a erally followed
E.zamp
The procedure of Example 10 was gen
to produce a wet powder, edible, clear, film-forming
composition having the following composition:
C'_~m_oonent wt . s
Hydroxypropylmethyl cellulose 78.70
Sodium citrate 0.55
WO 92/11002 PCT/BJ~,'9;:;,i~,':r:' ~7
19
Polyvinyl pyrrolidone 15.70
Water 5.00
A dustless, free-flowing powder was produced.
Example 25
The procedure of Example 10 was generally
followed
to produce a wet powder, edible, clear, film-forming
composition having the following composition:
Comg~n~n~ Wt .
Hydroxypropylmethyl cellulose 90.20
Tetrasodium ethylene diamine
tetraacetate 0.53
Polyethylene glycol 4.50
Water 4.70
A dustless, free-flowing powder was produced.
1S E~~ple 26
The procedure of Example 10 was generally
followed
to produce a wet powder, edible, clear, film-forming
composition having the following composition:
Compon_p, nt Wt-
Hydroxypropylmethyl cellulose 95.0
Water 5.0
A dustless, free-flowing powder was produced.
sample 27
The procedure of-~Eaample 10 was generally
followed
2S to produce a wet powder, edible, clear, film-forming
composition having the following composition:
Co~ponent
Hydroxypropylmethyl cellulose 90.0
Sodium citrate O.A
Polyethylene glycol 6.0
Water 3.6
A dustless, free-flowing powder was produced.
Example 2 8
The procedure of Example 1~ was generally
followed
i
~'~~"f 7_ )~ :'' "~ e'!'.
WO 92/11002 '~ ~ ~ ~ n '~ ;~ . . ..
to produce a wet powder, edible, clear, film-forming
composition having the following composition:
Component Wt.%
Hydroxypropylmethyl cellulose 45.75
5 Modified starch ("Purity
Gum 59", National Starch) 45.75
Sodium citrate 0.50
water ~ 8.00
A dustless, free-flowing powder was produced.
10 In view of the above, it will be seen that the
several objects of the invention are achieved and other
advantageous results attained.
As various changes could be made in the above
methods and products without departing from the scope of the
15 invention, it is intended that all matter contained in the
above description shall be interpreted as illustrative and
not in a limiting sense.
