U.S. patent application number 11/453873 was filed with the patent office on 2006-10-26 for high-amylose starch.
This patent application is currently assigned to ROQUETTE FRERES. Invention is credited to Domenico Carbone, Ernesto Fossati, Claude Quettier, Giovanni Semino.
Application Number | 20060240099 11/453873 |
Document ID | / |
Family ID | 8861526 |
Filed Date | 2006-10-26 |
United States Patent
Application |
20060240099 |
Kind Code |
A1 |
Carbone; Domenico ; et
al. |
October 26, 2006 |
High-amylose starch
Abstract
The subject of the present invention is a process for preparing
pregelatinized high amylose starch, having the steps consisting of:
forming a suspension comprising a high amylose starch and water;
subjecting the suspension to steam jet cooking at a temperature of
between 125 and 135.degree. C. so as to obtain a pregelatinized
high amylose starch paste; cooking and drying the pregelatinized
starch paste on a drum dryer at a pressure of between 2 and 10 bar,
so as to obtain a pregelatinized high amylose starch. A
pregelatinized high amylose starch is also disclosed having an
apparent density of less than 0.4 g/ml for a mean particle size of
100 micrometres.
Inventors: |
Carbone; Domenico;
(Pasturana, IT) ; Quettier; Claude; (Erquinghem
Lys, FR) ; Semino; Giovanni; (Cassano Spinola,
IT) ; Fossati; Ernesto; (Novi Ligure, IT) |
Correspondence
Address: |
YOUNG & THOMPSON
745 SOUTH 23RD STREET
2ND FLOOR
ARLINGTON
VA
22202
US
|
Assignee: |
ROQUETTE FRERES
LESTREM
FR
|
Family ID: |
8861526 |
Appl. No.: |
11/453873 |
Filed: |
June 16, 2006 |
Related U.S. Patent Documents
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Application
Number |
Filing Date |
Patent Number |
|
|
10105661 |
Mar 25, 2002 |
|
|
|
11453873 |
Jun 16, 2006 |
|
|
|
Current U.S.
Class: |
424/456 ;
514/60 |
Current CPC
Class: |
C08B 30/14 20130101;
A23G 3/346 20130101; A23L 27/79 20160801; A23G 3/346 20130101; A23G
2200/06 20130101; A61K 9/4816 20130101; A61K 9/286 20130101; A23G
2200/06 20130101; A23B 7/16 20130101 |
Class at
Publication: |
424/456 ;
514/060 |
International
Class: |
A61K 31/718 20060101
A61K031/718; A61K 9/64 20060101 A61K009/64 |
Foreign Application Data
Date |
Code |
Application Number |
Mar 26, 2001 |
FR |
01 04023 |
Claims
1. A pregelatinized high amylose starch, having an apparent density
of less than 0.4 g/ml for a mean particle size of 100
micrometres.
2. A soft gelatin capsule comprising the starch according to claim
1.
3. A hard gelatin capsule comprising the starch according to claim
1.
4. A pharmaceutical, dietary or agricultural solid form film-coated
with the starch according to claim 1.
5. An edible film comprising a flavouring and/or an active
ingredient having a solubility in water of less than 5% by weight,
comprising the starch according to claim 1.
6. Molecules having a solubility in water of less than 5% by
weight, wherein said molecules are encapsulated with the starch
according to claim 1.
7. A flavoured film or film comprising an active ingredient which
is weakly soluble in water, comprising a pregelatinized high
amylose starch according to claim 1.
8. The film according to claim 7, comprising, on a dry matter
basis, 5% to 40% of stabilized pregelatinized high amylose
starch.
9. The film according to claim 8, comprising, on a dry matter
basis, 5% to 25% of stabilized pregelatinized high amylose
starch.
10. A pregelatinized high amylose starch, having an apparent
density of less than 0.4 g/ml for a mean particle size of 100
micrometers, prepared by forming a suspension comprising a high
amylose starch and water; subjecting said suspension to steam jet
cooking at a temperature of between 125.degree. C. and 135.degree.
C. so as to obtain a pregelatinized high amylose starch paste;
drying said pregelatinized starch paste on a drum dryer at a
pressure of between 2 bar and 10 bar, so as to obtain a
pregelatinized high amylose starch.
11. A soft gelatin capsule comprising the starch according to claim
10.
12. A hard gelatin capsule comprising the starch according to claim
10.
13. A pharmaceutical, dietary or agricultural solid form
film-coated with the starch according to claim 10.
14. An edible film comprising a flavouring and/or an active
ingredient having a solubility in water of less than 5% by weight,
comprising the starch according to claim 10.
15. Molecules having a solubility in water of less than 5% by
weight, wherein said molecules are encapsulated with the starch
according to claim 10.
16. A flavoured film or film comprising an active ingredient which
is weakly soluble in water, comprising a pregelatinized high
amylose starch according to claim 10.
17. The film according to claim 16, comprising, on a dry matter
basis, 5% to 40% of stabilized pregelatinized high amylose
starch.
18. The film according to claim 17, comprising, on a dry matter
basis, 5% to 25% of stabilized pregelatinized high amylose
starch.
19. A pregelatinized high amylose starch, having an apparent
density of less than 0.4 g/ml for a mean particle size of 100
micrometres, wherein the high amylose starch has an amylose content
greater than 50%.
20. An edible film comprising a flavouring and/or an active
ingredient having a solubility in water of less than 5% by weight,
comprising the starch prepared by the process according to claim
19.
Description
FIELD OF THE INVENTION
[0001] The subject of the invention is a novel process for
preparing pregelatinized high-amylose starches.
[0002] Its subject is also the starches obtained by this
process.
BACKGROUND OF THE INVENTION
[0003] Pregelatinized starches are generally prepared by thermal,
chemical or mechanical techniques which can cause swelling of the
starch granules so that they are soluble in cold water.
[0004] The preferred techniques are spray-drying, cooking on a drum
or extrusion. Autoclaving or indirect heating on a heat exchanger
are cooking processes which tend to produce complex colloidal
dispersions consisting of intact, fragmented and swollen
granules.
[0005] It is well known that high amylose starches, that is to say
which have more than 50% by weight of amylose, are particularly
difficult to disperse and require high cooking temperatures.
[0006] The document U.S. Pat. No. 3,086,890 describes a process for
preparing pregelatinized amylose. This process consists in
autoclaving at 191.degree. C., under pressure, a solution of
amylose containing at most 25% by weight of dry matter, and then
drum-drying at 110-200.degree. C. The powders obtained are
amorphous and form irreversible gels after dispersion. Their
apparent density is high, that is to say generally greater than 0.4
g/ml.
[0007] The document U.S. Pat. No. 3,607,394 describes a process for
the pregelatinization of starches having amylose contents of less
than 60% by weight. This process consists in cooking the starch at
149.degree. C., followed by drum-drying, spray-drying or another
type of drying means.
[0008] The document EP 0 366 898 describes a coupled
cooking/spray-drying process which makes it possible to obtain
amorphous products, which are practically free of retrogradation,
and which have an apparent density greater than that of an
identical starch which has been subjected to the same process but
in two separate stages, that is an apparent density greater than
0.45 g/ml. The cooking of high amylose starches is carried out on a
jet cooker at 143.degree. C. and the spray-drying is carried out
with an inlet air temperature of 220.degree. C. This document
presents, in FIG. 7, a comparison of various prior art
pregelatinized starches.
[0009] Starting from this teaching, the applicants have now found,
after long research studies, that it was possible to prepare a
pregelatinized high amylose starch using a particular process
leading to products of low apparent density while working at not
very high temperatures, which none of the prior art techniques made
it possible to obtain.
OBJECTS AND DETAILED DESCRIPTION OF THE INVENTION
[0010] The subject of the invention is therefore a process for
preparing pregelatinized high amylose starch, characterized in that
it comprises the steps consisting of: [0011] forming a suspension
comprising a high amylose starch and water; [0012] subjecting the
said suspension to steam jet cooking at a temperature of between
125 and 135.degree. C. so as to obtain a pregelatinized high
amylose starch paste; [0013] drying the said pregelatinized starch
on a drum dryer at a pressure of between 2 and 10 bar, so as to
obtain a pregelatinized high amylose starch.
[0014] The pregelatinized high amylose starch obtained may then be
recovered and ground so as to obtain a powder having a particle
size which is chosen according to the uses which will be
subsequently made thereof.
[0015] The expression high amylose starches for the purposes of the
present invention denotes starches having an amylose content
greater than or equal to 50% by weight, and preferably of between
50 and 80% by weight, obtained from any plant origin, such as in
particular maize, potato, cassava.
[0016] Preferably, the process according to the invention uses a
maize starch such as, for example, EURYLON.RTM. marketed by the
Assignee.
[0017] The invention also applies to chemically or physically
modified high amylose starches. Preferably, the modified starch
will be chosen from the group consisting of acetylated,
hydroxypropylated, carboxy-methylated and fluidified starches, and
starch octenyl succinates.
[0018] According to a preferred variant of the process according to
the invention, an acetylated starch will be chosen.
[0019] The starch suspension is prepared at a dry matter content of
between 30 and 40% by weight so as to obtain a suspension in
water.
[0020] This suspension is then pregelatinized using a tuyere at the
outlet of which a steam counter-pressure is applied which is
sufficient to reach a cooking temperature for the suspension of
between 125 and 135.degree. C. while maintaining an acceptable
viscosity so that the flow rate of the milk coming out after
cooking is not too low. For example, a counter-pressure of the
order of 2 to 3 bar will be applied.
[0021] Surprisingly and unexpectedly, this cooking temperature is
necessary and sufficient to obtain good pregelatinized starch
solubility. The amylose fraction exists, according to the process
in accordance with the invention, in amorphous form, whereas the
prior art processes for cooking high amylose starches lead to an
amylose which has a high tendency to undergo retro-gradation.
[0022] The expression tuyere is understood to mean any direct steam
jet cooking device allowing instant cooking of a starch suspension
using pressurized steam.
[0023] A pregelatinized starch paste is obtained after this
cooking, which is then dried on a drum dryer.
[0024] Such an equipment makes it possible to reproduce, on one and
the same device, the cooking and drying stages by exploiting the
heat transferred from the surface of the drums heated with steam to
the starch paste. Steam pressure values of the order of 2 to 10 bar
will be applied, for example, according to the type of starch used.
The starch paste is uniformly spread in a thin film over the hot
surface of the drums by applying components. The drums are driven
in rotation, at a speed of the order of 5 to 8 revolutions per
minute. Thus, the cooking of the paste is continued, followed by
drying. The film formed is then scraped using a scraping blade so
as to detach a sheet which can then be ground.
[0025] The process according to the invention makes it possible to
homogeneously obtain pregelatinized high amylose starches without
the need for the use of very high temperatures as taught by the
prior art. The process according to the invention is particularly
advantageous because it uses simple techniques, with a lower energy
cost than the known techniques of spray-drying or autoclaving.
[0026] The pregelatinized high amylose starches according to the
invention are characterized by an apparent density of less than 0.4
g/ml for a mean particle size of 100 micrometres, which is
particularly surprising given the higher densities obtained
according to the prior art techniques and in particular those
described in patent EP-B1 0 366 898.
[0027] Their solubility in lukewarm water is good, in the region of
80%, whereas it is less than 30% when the tuyere cooking stage is
eliminated.
[0028] These starches have, in addition, various applicative
advantages such as, in particular, a good compression capacity, and
in particular very good capacities to form a film. This capacity is
particularly advantageous for film coating tablets in particular,
but also for numerous other applications requiring the formation of
a barrier to moisture and to air. To the knowledge of the
applicants, such pregelatinized high amylose starches capable of
having film-forming properties did not exist on the market. The
subject of the invention is therefore, in addition, the use of
pregelatinized high amylose starches for the manufacture of soft
gelatin capsules or of hard gelatin capsules, as well as for the
coating of solid forms in pharmacy, human foods, animal foods,
agrochemistry or plant substances such as seeds.
[0029] The subject of the invention is also the use of high amylose
starches obtained according to the invention for the preparation of
freshening films, also called flavour sheets. These flavour sheets
are small squares of edible films, which are very fine, highly
flavoured, and used as breath fresheners by dissolving rapidly in
the buccal cavity. The applicants have observed that in addition to
the remarkable film-forming properties of the starches according to
the invention, the latter had an advantageous capacity to
encapsulate molecules with low solubility in water, such as
flavourings or certain active ingredients. Indeed, during the
formulation of such films based on film-forming polymers, when
about 5% of flavouring or of active ingredient which are weakly
soluble in water are added to the film-forming preparation, a total
phase separation occurs during the spreading of the film, between
the hydrophobic molecules and the other components. The
film-forming solution is pushed to the sides of the band of film,
whereas the centre is only composed of flavouring or of active
ingredient. The film obtained therefore does not constitute a
homogeneous thin layer. The addition, before incorporation of the
flavouring, of a pregelatinized high amylose starch according to
the invention allows, surprisingly and unexpectedly, inclusion of
the flavourings or active ingredients which are weakly soluble in
water, on the one hand, and an excellent film quality, on the other
hand. Without wishing to be bound to any theory, the applicants are
of the opinion that this encapsulation property is linked to the
amorphous state of the precooked amylose according to the process
in accordance with the invention, given that the precooked high
amylose starches according to the prior art processes do not
possess this encapsulation property. The film obtained has the
desired properties, namely good solubility, adequate mechanical
properties, strong flavouring and no adherence between each
film-during packaging.
[0030] Thus, an edible film which is highly flavoured or which
comprises an active ingredient which is weakly soluble in water,
characterized in that it comprises a pregelatinized high amylose
starch according to the invention, constitutes, to the knowledge of
the applicants, a novel industrial product. The expression "weakly
soluble in water" is understood to mean, according to the present
invention, flavourings or active ingredients which have a
solubility in water of less than 5% by weight.
[0031] According to a preferred embodiment of the film according to
the invention, the latter comprises, on a dry matter basis, 5 to
40%, preferably 5 to 25%, of pregelatinized high amylose starch
according to the invention. According to a still more preferred
embodiment of the invention, the said pregelatinized high amylose
starch is stabilized, for example, by acetylation or
hydroxypropylation.
[0032] The film comprises, in addition, any other film-forming
polymer commonly used in practice, such as in particular high
amylopectin starches, modified or otherwise, high amylose starches,
modified or otherwise, standard or special maltodextrins,
film-forming polysaccharides and proteins such as gelatin,
pullulan, plant gums, gluten.
[0033] According to a preferred variant, the edible film comprises
5 to 40% of pregelatinized high amylose starch according to the
invention and 40 to 80% of high amylopectin starch. The balance for
100% consists of flavourings, active ingredients, sweeteners, one
or more humectants and optionally colourings. The final water
content of the films according to the invention is generally about
12%.
[0034] The expression high amylopectin starch is understood to mean
the so-called waxy starches, derived in particular from maize or
potato.
[0035] According to a still more preferred variant, the said film
comprises, on a dry matter basis, 5 to 40%, preferably 5 to 25%, of
pregelatinized high amylose starch according to the invention, and
40 to 80%, preferably 40 to 70%, of waxy starch fluidified by the
acid route.
[0036] A waxy starch derived from maize fluidified by techniques
known-to persons skilled in the art would be preferably chosen.
[0037] Of course, the film according to the invention may be used
as it is as a flavour sheet for freshening the breath, but it may
also be used for the film-coating of various supports, in
particular dietary or pharmaceutical supports. There may be
mentioned, without limitation, the film-coating of tablets,
confectioneries, or any other support.
[0038] The advantageous properties of encapsulation of substances
weakly soluble in water of the starches according to the invention
may also be exploited in any other type of application requiring
such properties, in aqueous medium or in the dry state.
[0039] The invention will be understood more clearly on reading the
following examples, which are intended to be explanatory and
nonlimiting.
EXAMPLES
Example 1
[0040] High amylose starches, modified or otherwise, are prepared
according to a process comprising the following steps: [0041]
preparation of a suspension of starch and water [0042] cooking in a
tuyere [0043] drying on a drum dryer [0044] recovery of a
powder
[0045] In all cases, the initial starch is EURYLON.RTM.7 marketed
by the Assignee, having an amylose content of 70% by weight.
[0046] The various process parameters are presented in Table 1, as
well as the apparent densities and the mean particle sizes of the
various products obtained. The apparent density is measured
according to the pharmaceutical technical method 2.9.16 of the
European Pharmacopoeia, 3rd edition. The mean particle size is
calculated from the particle size measured by sieving on successive
sieves of 500, 315, 200, 150, 100 and 50 micrometres.
[0047] The displacement density is measured according to the method
described in patent EP-B1 0 366 898. TABLE-US-00001 TRIAL 4 TRIAL 6
TRIAL 2 TRIAL 3 EURYLON .RTM. 7 TRIAL 5 EURYLON .RTM. 7 TRIAL 1
EURYLON .RTM. 7 EURYLON .RTM. 7 OCTENYL EURYLON .RTM. 7 FLUIDIFIED
EURYLON .RTM. 7 ACETYL ACETYL SUCCINATE HYDROXYPROPYL ACIDIC DRY
MATTER (%) 33.5 33.4 33.4 38 35.4 39 TUYERE TEMPERATURE 130 135 135
133 135 135 (.degree. C.) TUYERE 2.67 3.1 3.1 2.92 3.1 3.1
COUNTERPRESSURE (Bar) DRUM ROTATION SPEED 6.5 7 8 6.5 7 6.5
(revolutions/min) DRUM PRESSURE (Bar) 10 10 2 10 10 10 MEAN
PARTICLE SIZE 88.2 101.2 100.8 100.6 100.6 100.4 (.mu.m) APPARENT
DENSITY 0.31 0.22 0.23 0.34 0.16 0.37 (g/ml) DISPLACEMENT 1.26 1.26
1.2 1.6 1.05 1.95 DENSITY (g/ml)
Example 2
[0048] In order to illustrate the film-forming properties, the
product obtained according to trial No. 3 of the preceding example
is solubilized in hot water (70-80.degree. C.), with mechanical
stirring, at 15% of dry matter. The Brookfield viscosity is 4 000
mPa s at 70.degree. C. and 5 000 mPas s at 60.degree. C.
[0049] This solution is placed on a polyethylene support over a
thickness of 45.7 micrometres.
[0050] The solution thus deposited is dried at room temperature,
and gives a rigid film, which is nonbrittle, and which is insoluble
in water.
[0051] This film can give rise to very numerous applications, since
it can serve to coat all types of solid forms which it is desired
to protect, whether they are pharmaceutical (tablets, gelatin
capsules), dietary (fries, tart bases, confectioneries) or
agricultural (seeds, granules).
[0052] These film-forming properties may also be applied in the
manufacture of soft gelatin capsules or hard gelatin capsules.
Example 3
[0053] Flavour sheets are prepared according to the following
procedure:
[0054] Formula TABLE-US-00002 Composition of Quantity Composition
of the suspension used the film on a (%) (g) dry basis (%)
Fluidified waxy 27.75 138.75 55.5 starch (CLEARGUM .RTM.CB90) High
amylose 4.60 23.00 9.2 starch according to trial 2 example 1 Mint
flavour 2.50 12.50 5.0 SILESIA Glycerol 15.0 75.0 30.0 Sodium 0.15
0.75 0.3 saccharinate Water 50.0 250.0 -- Total 100 500 100
[0055] In a jacketed stainless-steel bowl, disperse the
CLEARGUM.RTM. in water, the glycerol and the saccharinate. Heat to
90.degree. C. [0056] Pour into the bowl of a KENWOOD mixer, add the
pregelatinized high amylose starch and the flavouring. Mix for 1
minute at the minimum speed (solution S). [0057] Pour the solution
S into the stainless-steel bowl and heat to 85.degree. C., degas
the mixture as much as possible. [0058] When the mixture is at
85.degree. C., form a film on a plastic plate (thickness of paste
=1.5 mm) with an automatic film applicator (bar-coater B-2105, RK
printcoat) equipped with a scale preheated to 60.degree. C. [0059]
Allow to dry in an oven at 20.degree. C. and 80% relative humidity
for 2 days and then end the drying at 20.degree. C. under an
uncontrolled atmosphere.
[0060] The film thus obtained, which is highly flavoured, is very
soluble, supple and flexible, nonbrittle and not cracked, regular
and homogeneous as regards the distribution of the flavour,
transparent. It does not stick on contact with other films during
prolonged storage. It can therefore be easily used as freshening
flavour sheet, or in order to wrap or coat any type of support, in
particular a dietary or pharmaceutical support.
[0061] A film prepared in the same manner but without incorporating
starch according to the invention is completely heterogeneous in
its centre and impossible to detach from its support in the form of
a uniform sheet.
* * * * *