U.S. patent application number 10/542049 was filed with the patent office on 2006-03-16 for process for the produciton of cross-linked gelatin beadlets.
Invention is credited to Sylvain Diguet, Torsten Huber, Johann Ulm.
Application Number | 20060057214 10/542049 |
Document ID | / |
Family ID | 33040921 |
Filed Date | 2006-03-16 |
United States Patent
Application |
20060057214 |
Kind Code |
A1 |
Diguet; Sylvain ; et
al. |
March 16, 2006 |
Process for the produciton of cross-linked gelatin beadlets
Abstract
The invention provides a process for the production of
cross-linked beadlets containing one or more active ingredients
selected from the group of a fat-soluble vitamin active material, a
carotenoid and a polyunsaturated fatty acid, the process comprising
treating a dry particulate form at a temperature in the range of
from 90.degree. C. to 140.degree. C. for a time period of from 30
seconds to 30 minutes or from 1 minute to 10 minutes or from 3
minutes to 7 minutes.
Inventors: |
Diguet; Sylvain;
(Hagenthal-le-haut, FR) ; Huber; Torsten; (Magden,
CH) ; Ulm; Johann; (Oberwil, CH) |
Correspondence
Address: |
NIXON & VANDERHYE, PC
901 NORTH GLEBE ROAD, 11TH FLOOR
ARLINGTON
VA
22203
US
|
Family ID: |
33040921 |
Appl. No.: |
10/542049 |
Filed: |
March 18, 2004 |
PCT Filed: |
March 18, 2004 |
PCT NO: |
PCT/EP04/02821 |
371 Date: |
July 13, 2005 |
Current U.S.
Class: |
424/489 ;
514/560; 514/725; 514/763 |
Current CPC
Class: |
A61K 9/167 20130101;
A61K 9/1694 20130101; A61K 9/1658 20130101; A61K 9/1623 20130101;
A61P 3/02 20180101 |
Class at
Publication: |
424/489 ;
514/560; 514/763; 514/725 |
International
Class: |
A61K 9/14 20060101
A61K009/14; A61K 31/015 20060101 A61K031/015; A61K 31/07 20060101
A61K031/07; A61K 31/202 20060101 A61K031/202 |
Foreign Application Data
Date |
Code |
Application Number |
Mar 27, 2003 |
EP |
03007009.8 |
Claims
1-11. (canceled)
12. A process for the production of cross-linked beadlets
containing one or more active ingredients selected from the group
of a fat-soluble vitamin active material, a carotenoid and a
polyunsaturated fatty acid, which comprises the steps of forming an
emulsion containing the active ingredients, an emulsifier and a
reducing sugar, converting the emulsion to droplets, coating the
droplets with finely dispersed powder, separating a dry particulate
form from the remaining finely dispersed powder, and heat treating
said particulate form, characterized in that the dry particulate
form is heat treated at a temperature in the range of from
90.degree. C. to 140.degree. C. for a time period of from 30
seconds to 30 minutes or from 1 minute to 10 minutes or from 3
minutes to 7 minutes in such a way that the final beadlet forms
have a core and a surface region, wherein the core region contains,
in a high concentration, the active.about.ingredients and the
surface region contains less than 10% of the total active
ingredient content.
13. The process according to claim 12 wherein the fat-soluble
vitamin active material is selected from vitamin A, vitamin D and
vitamin E, the carotenoid is selected from .beta.-carotene,
lycopene, zeaxanthin, astaxanthin, lutein, capsanthin and
cryptoxanthin and the polyunsaturated fatty acid is selected from
arachidonic acid, eicosapentaenoic acid, docosahexaenoic acid and
.gamma.-linolenic acid and triglycerides and ethylesters
thereof.
14. The process according to claim 13 wherein the concentration of
the fat-soluble vitamin active material, the carotenoid and the
polyunsaturated fatty acid is selected from a total concentration
in the range of from 500,000 IU vitamin Mg beadlet to 1,500,000 IU
vitamin A/g beadlet, in the range of from 100,000 IU vitamin D/g
beadlet to 500,000 IU vitamin D/g beadlet, in the range of from 50%
to 75% vitamin E, in the range of from 5% to 20% of carotenoid and
in the range of from 20% to 50% polyunsaturated fatty acid as
triglyceride.
15. The process according to claim 12 wherein as finely dispersed
powder calcium silicate is used.
16. The process according to claim 12 wherein the dry particulate
forms have a moisture content of less than 10%.
17. The process according to claim 12 wherein the heat treatment is
achieved in a batch or in a continuous process where the beadlet
residence time and temperature are controlled.
18. The process according to claim 12 wherein the beadlet is added
in a hot air or nitrogen stream having a temperature between 100
and 200.degree. C.
19. The process according to claim 12 wherein after addition of the
dry particulate form the temperature is raised in a time in the
range of from a few seconds to 1 minute above 100.degree. C.
20. The process according to claim 12 wherein heating takes place
at a maximum beadlet temperature in the range of from 110.degree.
C. to 140.degree. C.
21. A cross-linked beadlet form having a core and a surface region,
wherein the core region contains, in a high concentration, one or
more active ingredients selected from the group of a fat-soluble
vitamin active material, a carotenoid and a polyunsaturated fatty
acid, and the surface region contains less than 10% or less than 5%
of the total active ingredient content.
22. A cross-linked beadlet form containing one or more active
ingredients selected from the group of Vitamin A in a total
concentration in the range of from 800,000 IU vitamin A/g beadlet
to 1,500,000 IU vitamin Mg beadlet, in a total concentration in the
range of from 100,000 IU vitamin D/g beadlet to 500,000 IU vitamin
D/g beadlet, vitamin E in a total concentration in the range of
from 50% to 75%, a carotenoid in a total concentration in the range
of from 5 to 20% and a polyunsaturated fatty acid in a total
concentration in the range from 5 to 50%, wherein the surface
region contains less than 10% or less than 5% of the total active
ingredient content.
23. The cross-linked beadlet form according to claim 22 having the
following components: 30% to 45% of vitamin A, 0% to 2% of vitamin
D.sub.3, 5% to 15% of
6-ethoxy-1,2-dihydro-2,2,4-trimethylquinoline, as emulsifier 25% to
35% of gelatine, as reducing sugar 5% to 10% of fructose, 2% to 10%
of glycerine, 5% to 10% of calcium silicate, 0% to 25% of corn
starch, 0% to 1% of edible fat, and water.
Description
FIELD OF THE INVENTION
[0001] The present invention relates to a process for the
production of beadlets with a high concentration of an active
ingredient selected from a fat soluble vitamin, a carotenoid and a
polyunsaturated fatty acid, to the resulting beadlets and to
compositions containing them.
SUMMARY OF THE INVENTION
[0002] More particularly the invention provides a process for the
production of cross-linked beadlets containing one or more active
ingredients selected from the group of a fat-soluble vitamin active
material, a carotenoid and a polyunsaturated fatty acid, the
process comprising treating a dry particulate form at a temperature
in the range of from 90.degree. C. to 140.degree. C. for a time
period of from 30 seconds to 30 minutes or from 1 minute to 10
minutes or from 3 minutes to 7 minutes.
DETAILED DESCRIPTION
[0003] Examples of a fat-soluble vitamin active material include
vitamin bearing oils, provitamins and pure or substantially pure
vitamins, both natural and synthetic, or chemical derivatives
thereof and mixtures thereof. Of particular interest is a vitamin
selected from the group of vitamins A, D, E and K, and derivatives
thereof. For example, the term "Vitamin E" includes synthetically
manufactured tocopherols or a mixture of natural tocopherols.
Examples of vitamin derivatives include vitamin A acetate, vitamin
A palmitate and vitamin E acetate. An example for a vitamin
D-active material is vitamin D.sub.3. As a particular example, the
process of the present invention may result in a beadlet containing
a vitamin A-active material and a vitamin D-active material, e.g.
vitamin A and vitamin D.sub.3.
[0004] In one embodiment the process of the invention may involve
Vitamin A as fat-soluble vitamin active material in a total
concentration in the range of from 500,000 IU vitamin A/g beadlet
to 1,500,000 IU vitamin A/g beadlet, in the range of from 750,000
IU vitamin A/g beadlet to 1,500,000 IU vitamin A/g beadlet, or in
the range of from 750,000 IU vitamin A/g beadlet to 1,300,000 IU
vitamin A/g beadlet, e.g. vitamin A may be present in the beadlet
in a total concentration of 500,000.+-.35,000 IU active
ingredient/g beadlet, 750,000.+-.35,000 IU active ingredient/g
beadlet, of 1,000,000.+-.35,000 IU active ingredient/g beadlet, or
of 1,100,000.+-.35,000 IU active ingredient/g beadlet. Vitamin D as
fat-soluble vitamin active material maybe present in the range of
from 100,000 IU vitamin D/g beadlet to 500,000 IU vitamin D/g
beadlet or in the range of from 100,000 IU vitamin D/g beadlet to
200,000 IU vitamin D/g beadlet, vitamin E as fat-soluble vitamin
active material may be present in the range of from 50% to 75%
vitamin E.
[0005] Examples for a carotenoid include .beta.-carotene, lycopene,
zeaxanthin, astaxanthin, lutein, capsanthin and cryptoxanthin.
[0006] In one embodiment the process of the invention may involve a
carotenoid in a total concentration in the range of from 5% to 20%,
in the range of from 5% to 15%, or in the range of from 7% to
15%.
[0007] Examples for a polyunsaturated fatty acid, as triglyceride
and/or ethylester, include arachidonic acid, eicosapentaenoic acid,
docosahexaenoic acid and .gamma.-linolenic acid and/or
ethylester.
[0008] In one embodiment the process of the invention may involve a
polyunsaturated fatty acid as triglyceride in a total concentration
in the range of from 20% to 50%, in the range of from 25% to 40%,
or in the range of from 28% to 38%.
[0009] The dry particulate forms used in the process of the present
invention may be prepared by any procedure known to the skilled
artisan, e.g. by forming an aqueous emulsion containing the active
ingredient, an emulsifier, a texturing agent and a reducing sugar,
followed by converting the emulsion to a dry particulate form
containing the non-aqueous constituents of said emulsion.
[0010] Examples for an emulsifier are gelatine and ascorbyl
palmitate. Gelatine is an emulsifier which at the same time
functions as a texturing agent. Any gelatine which has a "bloom" in
the range of practically zero to about 300 can be employed in the
practice of the present invention. Both Type A and Type B gelatine
can be employed. The preferred gelatine used is Bloom 140, but
gelatine Bloom 30 or Bloom 75 would be possible as well. In the
presence of gelatine no additional texturing agent maybe
necessary.
[0011] The concentration of the emulsifier depends on the kind of
emulsifier used, e.g. gelatine maybe present in a concentration in
the range of from 25% to 35%, or less.
[0012] Examples for a texturing agent beyond gelatine include
carrageenan, modified starch, modified cellulose, xanthan gum,
acacia gum, pectins, guar, caroub gums, maltodextrines and
alginates.
[0013] The concentration of the texturing agent depends on the kind
of texturing agent used and maybe, e.g., in the range of from 0% to
15%.
[0014] Examples for a reducing sugar are fructose, glucose,
lactose, maltose, xylose, arabinose, ribose and sucrose. One type
of sugar maybe used or a mixture of two or more sugars. The
reducing sugar may be added as such or in the form of a syrup, e.g.
fructose or glucose syrop.
[0015] The concentration of the reducing sugar depends on the kind
of reducing sugar used and maybe, e.g., in the range of from 2% to
10%, or in a ratio of gelatine:sugar in the range of from 3:1 to
7:1, e.g. 5:1.
[0016] Small quantities of other ingredients may be incorporated
including antioxidants like
6-ethoxy-1,2-dihydroxy-2,2,4-trimethylquinoline (ethoxyquine),
3,5-di-tertiary-4-butyl hydroxytoluene (BHT)and
3-tertiarybutyl-hydroxyanisole (BHA), humectants, such as glycerol,
sorbitol, polyethylene glycol, propylene glycol, extenders and
solubilizers.
[0017] As a typical example gelatine and a suitable sugar may be
dissolved in water previously mixed with glycerin. The dissolution
may last at 65-70.degree. C. for, e.g., about 30 minutes. Then,
e.g., the vitamin A with the antioxidant may be added and
emulsified. The pre-emulsification may be done with a colloid mill,
e.g., based on a rotor/stator principle. The pre-emulsification may
be hold for between 15 and 30 minutes at a rotation speed of the
rotor between 500 and 1500 rpm and may then pass through a high
pressure homogeniser resulting in a conversion of the emulsion to
fine droplets.
[0018] In one example the conversion of emulsion droplets to "set
up" particles may be attained by introducing a spray of emulsion
droplets into an agitated cloud or suspension in air of the
particles of the finely dispersed powder, e.g. by forcing the
emulsion through a revolving spray head into a suspension in air of
the powdered material, contained in and agitated by a revolving
cylindrical drum, the drum and the spray head rotating in opposite
directions so that the cloud or suspension of the powder in air is
swirling in a sense of rotation opposite to the entering emulsion
spray.
[0019] Examples of the finely dispersed powder used in the process
to collect/coat the droplets of the emulsion include
polysaccharides such as starch and modified starch, and calcium
silicate alone or a mixture of calcium silicate with one of the
following mixture components: microcrystalline cellulose, magnesium
silicate, magnesium oxide, stearic acid, calcium stearate,
magnesium stearate, hydrophilic silicic acid and kaolin. Coatings
which consist of calcium silicate alone are preferred. The calcium
silicate may be present wholly or partially in the form of the
hydrate.
[0020] The calcium silicate particles are especially suitable when
they have a size of less than 0.2 .mu.m, especially less than 0.1
.mu.m, and a specific surface of at least about 80 m.sup.2/g to
about 180 m.sup.2/g, preferably of about 95 m.sup.2/g to 120
m.sup.2/g, and are agglomerated to aggregates having an average
size of about 5-30 .mu.m, preferably 5-20 .mu.m. The SiO.sub.2/CaO
ratio lies between 1.65 and 2.65.
[0021] In coatings which consist of calcium silicate alone, the
amount of calcium silicate may be in the range of from 2 wt. % to
12 wt. %, preferably in the range of from 4 wt. % to 9 wt. %.
[0022] In coatings consisting of a mixture of calcium silicate with
one or more of the aforementioned mixture components, the amount of
the calcium silicate mixture may be in the range of from 5 wt. % to
25 wt. %.
[0023] Optionally, the resulting dry particulate forms may be
separated from the remaining finely dispersed powder. This may be
accomplished by operations which are conventional per se,
including, e.g. simply to feed the mixture of powder and dry
particulate forms to a shaking screen of a size selected to retain
the dry particulate forms while passing the collecting powder.
[0024] For further processing those dry particulate forms
containing the active material are preferred having a moisture
content of less than 10% and preferably between about 4 to 6
percent. If the moisture content is higher the dry particulate
forms maybe dried to the desired moisture content by various
methods, e.g. by exposing them to air at room temperature or by
moderate heating in a drying oven at 37.degree. C. to 45.degree.
C.
[0025] The heat treatment may, e.g., be achieved in a batch or in a
continuous process where the beadlet-residence time and temperature
are controlled.
[0026] In the case of a fluid bed process, the beadlet is added
either at the beginning in the case of the batch process or
constantly in the case of a continuous fluid bed in a hot air or
nitrogen stream having a temperature between 100 and 200.degree.
C.) preferably between 130-160.degree. C. The beadlet temperature
is raised in a few second to one minute above 100.degree. C.
enabling a quick and efficient reaction. The beadlet is ready after
5 to 10 minutes. The beadlet is cooled at the end of the
treatment.
[0027] In the case of a continuous flash treatment, the beadlet is
fed continuously into a hot gas stream having a temperature between
100 and 200.degree. C., preferably between 130-160.degree. C. The
beadlet can be moved by mechanical stirring, e.g., above 300 rpm.
The wall of the vessel used to make this thermal treatment can also
be heated to a temperature in the range of from 110 to 180.degree.
C. The desired crosslinking of the beadlet may be reached in a time
in the range of from 30 seconds to 10 minutes or from 1 minute to
10 minutes, with a maximum beadlet temperature in the range of from
90.degree. C. to 140.degree. C., preferably from 105.degree. C. to
125.degree. C.
[0028] The beadlet forms resulting from the inventive process have
a core and a surface region, wherein the loss of active ingredients
in the surface region is reduced, and are also an object of the
present invention.
[0029] Therefore, the present invention further provides a beadlet
form having a core and a surface region, wherein the core region
contains, in a high concentration, one or more active ingredients
selected from the group of a fat-soluble vitamin active material, a
carotenoid and a polyunsaturated fatty acid, and the surface region
contains less than 10% of the total active ingredient content,
preferably less than 5% of the total active ingredient content.
[0030] In one embodiment the present invention provides a beadlet
form containing one or more active ingredients selected from the
group of Vitamin A in a total concentration in the range of from
800,000 IU vitamin A/g beadlet to 1,500,000 IU vitamin A/g beadlet
or in the range of from 950,000 IU vitamin A/g beadlet to 1,250,000
IU vitamin A/g beadlet, in a total concentration in the range of
from 100,000 IU vitamin D/g beadlet to 500,000 IU vitamin D/g
beadlet or in the range of from 100,000 IU vitamin D/g beadlet to
200,000 IU vitamin D/g beadlet, vitamin E in a total concentration
in the range of from 50% to 75%, a carotenoid in a total
concentration in the range of from 5 to 20% and a polyunsaturated
fatty acid in a total concentration in the range of from 5 to 50%,
wherein the surface region contains less than 10%. of the total
active ingredient content. In another embodiment the surface region
contains less than 5% of the total active ingredient content.
[0031] The beadlets are characterized by high stability and
potency. They exhibit high stability when pelletized, e.g. they
withstand the temperature, moisture and pressure of a feed
pelleting process without losing their physical integrity. They are
water insoluble and maintain their properties in relation to
bioavailability.
[0032] Typical examples of beadlets of the present invention may,
e.g. have the following components: 30% to 45% of vitamin A, 0% to
2% of vitamin D.sub.3, 5% to 15% of
6-ethoxy-1,2-dihydro-2,2,4-trimethylquinoline (EMQ), 25% to 35% of
gelatine, 5% to 10% of fructose, 2% to 10% of glycerine, 5% to 10%
of calcium silicate, 0% to 25% of corn starch, 0% to 1% of edible
fat, and water.
EXAMPLE 1
Preparation of Beadlets containing 1,000,000 IU Vitamin A/g Beadlet
Plus 200,000 IU Vitamin D.sub.3/g Beadlet
[0033] Approximately 90 parts of gelatine Bloom 140 and 18 parts of
fructose were dissolved in 313.2 parts of water (containing 23.2
parts of glycerin) by heating at 65.degree. C. 158 parts of Vitamin
A containing 24% ethoxyquin (assay 2.1 Mio. IU vitamin A per g) and
3.5 parts of vitamin D.sub.3 (assay 20 Mio. IU vitamin D.sub.3 per
g) were then mixed with the resulting matrix, followed by
pre-emulsification.
[0034] The beadlet was sprayed using as finely dispersed powder
calcium silicate. The average particle size of the beadlet was in
the range of from 200 .mu.m to 300 .mu.m.
[0035] The beadlet was divided into two groups: one group was
treated using a classical heated slow mixer without sufficient
control of the thermal history of the beadlet, and the other group
was treated by a fluidized bed, i.e. a batch process with an
apparatus where the temperature and residence time of the beadlet
can be controlled. The results are compared in the following table:
TABLE-US-00001 heated slow fluidized mixer bed Vitamin A content
after 1,025,000 1,050,000 crosslinking (IU/g) Vitamin A Loss (%)
3-4 0-1 Surface vitamin A (%) 8-10 1-2 Crosslinking grade (%) 76%
82%
[0036] In the fluidized bed the temperature was controlled between
100 and 115.degree. C. for 5 minutes. In the heated slow mixer, the
beadlet was heated for about 15 minutes at a temperature raising
from 90.degree. C. to 124.degree. C.
EXAMPLE 2
Preparation of Beadlets containing 1,000,000 IU Vitamin A/g
Beadlet
[0037] Approximately 100 parts of gelatine Bloom 140 and 20 parts
of fructose were dissolved in 308.2 parts of water (containing 13.2
parts of glycerin) by heating at 65.degree. C. 170 parts of Vitamin
A containing 24% ethoxyquin (assay 2.1 Mio. IU vitamin A per g)
were then mixed with the resulting matrix, followed by
pre-emulsification.
[0038] The beadlet was sprayed using as finely dispersed powder
calcium silicate. The average particle size of the beadlet was in
the range of from 180 .mu.m to 270 .mu.m.
[0039] The beadlet was divided into three groups: the first group
was treated using a classical heated slow mixer as in Example 1,
the second group was treated by a fluidized bed as in Example 1,
the third group was treated by a continuous flash treatment in
diluted phase wherein the flash treatment is ensured by a
combination of pneumatic transport and mechanical transport. The
results are compared in the following table: TABLE-US-00002 heated
slow fluidized flash mixer bed treatment Vitamin A content after
1,119,000 1,146,000 1,143,000 crosslinking (IU/g) Vitamin A Loss
(%) 3-4 0-1 0-1 Surface vitamin A (%) 8-10 2-2.5 3-5 Crosslinking
grade (%) 50-80 50-80 50-80
[0040] In the fluidized bed the temperature was controlled between
110 and 120.degree. C. for 5 minutes. In the flash treatment, the
beadlet was treated for 1 to 4 minutes at a temperature raising
from 115.degree. C. to 125.degree. C. In the heated slow mixer, the
beadlet was heated for about 20 minutes at a temperature raising
from 70.degree. C. to 124.degree. C.
EXAMPLE 3
Stability of Beadlets containing a High Concentration of Vitamin
A
[0041] Typical stability performance in terms of retention time
after a storage time of 4 weeks at 40.degree. C. and 75% rH for the
cross-linked beadlets of Example 1 and Example 2 are about 90-95%
which is comparable to standard cross-linked vitamin A forms
containing 500'00 IU vitamin A/g active ingredient.
EXAMPLE 4
Preparation of Beadlets containing 1,000,000 IU Vitamin A/g
Beadlet
[0042] Approximately 100 parts of gelatine Bloom 140 and 20 parts
of fructose were dissolved in 308.2 parts of water (containing 13.2
parts of glycerin) by heating at 65.degree. C. 170 parts of Vitamin
A containing 24% ethoxyquin (assay 2.1 Mio. IU vitamin A per g)
were then mixed with the resulting matrix, followed by
pre-emulsification.
[0043] The beadlet was sprayed using as finely dispersed powder
calcium silicate. The average particle size of the beadlet was in
the range of from 200 .mu.m to 300 .mu.m.
[0044] The beadlets of 3 lots were treated by a continuous flash
treatment in diluted phase wherein the flash treatment is ensured
by a combination of pneumatic transport and mechanical transport.
The results are compared in the following table: TABLE-US-00003 Lot
1 Lot 2 Lot 3 Vitamin A content after 1,064,808 1,051,641 1,077,224
crosslinking (IU/g) Vitamin A Loss (%) <1 <1 <1 Surface
vitamin A (%) 3.7 4.0 3.5 Crosslinking grade (%) 60-85 60-85
60-85
[0045] In the flash treatment, the beadlet was treated for 1 to 5
minutes at a temperature raising from 105.degree. C. to 115.degree.
C.
EXAMPLE 5
Stability of Beadlets containing a High Concentration of Vitamin
A
[0046] Typical stability performances in terms of retention time
after a storage time of 4 weeks at 40.degree. C. and 75% rH for the
cross-linked beadlets of Example 4 are about 95-100% which are
comparable to standard cross-linked vitamin A forms containing
500'00 IU vitamin A/g active ingredient.
EXAMPLE 6
Preparation of Beadlets containing 1,000,000 IU Vitamin A/g Beadlet
Plus 200,000 IU Vitamin D.sub.3/g Beadlet
[0047] Approximately 90 parts of gelatine Bloom 140 and 18 parts of
fructose were dissolved in 313.2 parts of water (containing 23.2
parts of glycerin) by heating at 65.degree. C. 158 parts of Vitamin
A containing 24% ethoxyquin (assay 2.1 Mio. IU vitamin A per g) and
3.5 parts of vitamin D.sub.3 (assay 20 Mio. IU vitamin D.sub.3 per
g) were then mixed with the resulting matrix, followed by
pre-emulsification.
[0048] The beadlet was sprayed using as finely dispersed powder
calcium silicate. The average particle size of the beadlet was in
the range of from 200 .mu.m to 300 .mu.m.
[0049] The beadlets of 3 lots were treated treated by a continuous
flash treatment in diluted phase wherein the flash treatment is
ensured by a combination of pneumatic transport and mechanical
transport. The results are compared in the following table:
TABLE-US-00004 Lot 1 Lot 2 Lot 3 Vitamin A content after 1,105,039
1,074,633 1,077,470 crosslinking (IU/g) Vitamin D3 content after
218,617 214,813 217,858 crosslinking (IU/g) Vitamin A Loss (%)
<1 <1 <1 Surface vitamin A (%) 4.7 4.7 4.6 Crosslinking
grade (%) 60-85 60-85 60-85
[0050] In the flash treatment, the beadlet was treated for 1 to 5
minutes at a temperature raising from 105.degree. C. to 115.degree.
C.
EXAMPLE 7
Stability of Beadlets containing a High Concentration of Vitamin A
and D3
[0051] Typical stability performances in terms of retention time
after a storage time of 4 weeks at 40.degree. C. and 75% rH for the
cross-linked beadlets of Example 6 are about 95-100% and about 100%
for vitamin A and D3 respectively, which are comparable to standard
cross-linked vitamin AD3 forms containing 500'00 IU vitamin A/g and
100'000 IU vitamin D3/g active ingredient.
* * * * *