EXCIPIENT FROM TRIGONELLA FOENUM-GRACEUM SEEDS AND
PROCESS FOR PREPARATION THEREOF
FIELD OF THE INVENTION
The present invention relates to an excipient obtained from Trigonellafoenum-graceum seeds and a
process for preparation thereof. The invention further relates to an excipient obtained from Trigonella
foenum-graceum seeds, comprising not less than 50% dietary fibers with ratio of insoluble dietary
fibers to soluble dietary fibers of about 0.2 to about 1 and protein content of not more than about 10
weight%. The invention also relates to the use of this excipient in various pharmaceutical or cosmetic
compositions and food, nutritional or dietary preparations.
BACKGROUND OF THE INVENTION
Trigonellafoenum-graceum commonly known as fenugreek is an herbaceous plant of the leguminous
family and is native to Western Asia, from where it has spread widely over Europe, the
Mediterranean and rest of Asia. It is one of the oldest cultivated plants and through ages has found
wide applications as a food, a food additive and as a traditional medicine in every region wherein it
has been cultivated. The leaves and both the ripe and unripe seeds of Trigonellafoenum-graceum are
used as vegetables. The seeds also function as a food preservative and are added to pickles, chutneys
and other similar food products. The ripe seeds have numerous applications in the traditional
medicine system of India. Fenugreek has been used in treating colic flatulence, dysentery, diarrhea,
dyspepsia with loss of appetite, chronic cough, dropsy, enlargement of liver and spleen, rickets, gout
and diabetes.
The fenugreek seed contains a central hard yellow embryo surrounded by a corneous and
comparatively large layer of white, semi-transparent endosperm. The endosperm is surrounded by a
tenacious, dark brown testa. The endosperm and testa are referred to as husk. In mature seeds the
majority of the endosperm cells are nonliving, the cytoplasmic content of which are occluded by the
store reserves viz galactomannan. Fenugreek seed contains a large number of compounds such as
volatile oil, fixed oils, proteins, carbohydrates, dietary fibers, hemicellulose, galactomannans,
cellulose, saponins, resins, pigments, vitamins, minerals and others.
Typical analysis results of fenugreek seeds are documented in the table 1 hereunder:
Table 1: Typical analysis of fenugreek seeds
CONSTITUENT PERCENTAGE
1. MOISTURE 9.0
2. ASH 3.2
3. LIPIDS 7.0
4. PROTEINS 26.0
5. STARCH 1.6
6 . FIBER 48.0
• Mucilage 20.0
• Hemicelluloses 17.3
• Cellulose 8.2
• Lignin 2.5
7. SAPONIN 4.8
8. TRIGONELLINE 0.37
(Source: THE WEALTH OF INDIA, CSIR GOVT. OF
Various seed components of Trigonella foenum-graceum along with the dietary fibers have an
important role in the treatment and management of several disorders such as obesity, coronary heart
disease, diabetes, piles, fissures, chronic constipation and diverticulitis. The saponins are reported to
contain active components that are anti-carcinogenic, anti-microbial and/or anti-oxidant. The dietary
fiber is the non-absorbable and indigestible fibrous portion, which is not assimilated by the body and
is non-caloric and has substantially no nutrition value. It includes both soluble and insoluble fibers.
Insoluble dietary fibers primarily comprise cellulose, lignin and some hemicelluloses; while soluble
dietary fiber comprises pectin, gums and some hemicelluloses.
Owing to the versatile functionality of the various seed components of Fenugreek, attempts have been
made to isolate these components using various processes. These processes mainly make use of
organic solvents and/or specialized equipments for extraction of the components. Majority of these
attempts emphasize upon isolation of fractions that include primarily soluble dietary fibers with high
protein content.
U.S. Patent 5,997,877 discloses a process for the fractionation of fenugreek seeds to provide various
fractions thereof including a soluble dietary fiber fraction, de-flavored fenugreek seed, high protein
fenugreek meal, dioscin and other saponins, along with fenugreek oleoresins. The process disclosed
herein comprises tempering the fenugreek seed to moisture content in the range of 14% to 22%;
flaking or milling the fenugreek seed; followed by solvent extraction and precipitation of the soluble
gum. In one aspect the flaked fenugreek seeds are treated with polar alcohols at high temperatures to
isolate oleoresin component prior to isolation of soluble dietary fiber; this process may however lead
to loss of some amount of dietary fibers. Further, the soluble dietary fibers are isolated by heating the
milled fenugreek over-fraction comprising endosperm and hull with water as a solvent at 60°C for 4
hours which may affect the quality of the final product as well as the viscosity of the dietary fiber
obtained. U.S. Patent 6,495,175 discloses a method employing two different solvent extraction stages
for obtaining substantially pure fixed oil, oleoresin and dietary fiber from Fenugreek seeds wherein
the first extraction isolates fixed oils and the second extraction isolates oleoresin to finally provide
dietary fibers that remain after extraction. Described herein is a special extraction system for better
efficiency. Further the process disclosed in this application utilizes grinding and sieving of the
fenugreek seeds for imparting higher surface area for better extraction which is well-known in the art.
Use of high temperature, solvents and specialized extractor during the extraction process, makes the
process very difficult on the commercial scale. Additionally, since the embryo is not separated from
the dietary fiber at the time of grinding or isolation, the fibers obtained have higher protein content,
which is not a desirable attribute for a pharmaceutical excipient.
U.S. Patent 5,658,571 discloses a process for preparing debitterised powder of the fenugreek seed.
Guar gum and bran are discussed to be blended with the debitterised powder of the seed of fenugreek
to prepare formulations that can be used as fiber supplements. The process for debitterization of
fenugreek seed disclosed involves the use of solvents and special jacketed extractor and therefore
tends to have similar disadvantages as discussed above. The debitterised powder comprises a total
dietary fiber of 48% by weight wherein the insoluble fiber is 28% by weight and the soluble fiber is
20% by weight. Further since the embryo is not separated from the dietary fiber during the
preparation process, the debitterised powder is likely to have higher protein content, which is again
not a desirable attribute for a pharmaceutical or food excipient. PCT Publication W099/25197A1
discloses a fenugreek seed material having reduced odor and taste. The method of preparing the
flaked/ground alcohol extracted fenugreek seed material, comprises the steps of: flaking a fenugreek
seed to form a fenugreek preparation, extracting soluble components from the fenugreek preparation
by extraction of the fenugreek preparation with an alcohol solvent at a cool extraction temperature to
produce fenugreek solid; treating the fenugreek solid to remove the alcohol solvent to produce a dry
solid; and grinding the dry solid into a powder to produce the fenugreek seed material. The process
disclosed herein results in a product having a high amount of protein (about 20 - 40%), which not
only reduces the amount of dietary fiber content in the end product but is also undesirable as a
pharmaceutical and food excipient.
PCT Publication WO01/74371A1 discloses fenugreek mucilages and galactomannans. The fenugreek
mucilages discussed herein are in the form of flour with grain size distribution less than ,
consisting of 60 weight % of oses, relative to the composition total weight, namely mannose,
galactose, glucose, arabinose, xylose, rhamnose, D-galacturonic acid with 50-55 weight % of oses
consisting of galactomannans, and 5 weight % of proteins. The galactomannans disclosed further
consist exclusively as oses, of mannose and galactose, with a mannose/galactose ratio of 1, 1.2. The
key feature of the invention is pulverization of non-lipid fraction of fenugreek seed at sub-zero
temperatures (-195 degrees) to improve the solubility of non-lipid fraction of fenugreek seed in the
extracting solvent. This requires a specialized facility to carry out such an operation thereby
increasing the cost of isolation of dietary fiber. U.S. Patent 5,847,109 discloses an isolated
galactomannan having at least 50 repeating units of mannose and galactose in a ratio of between 0.5-
1.0 and .8-1 .0, and having a protein content of less than 20 wt. %, a saponin content of less than 5
wt. %, and a lipid content of less than 1 wt. %. The process of isolation of galactomannan (soluble
fiber) described herein involves use of organic solvents and high temperatures as well as specialized
equipment. This process also involves treatment with polar alcohols that tend to reduce the yield of
the soluble dietary fiber. The process further involves reduction in protein content by using
chromatographic techniques that are difficult and expensive to carry out at commercial scale.
PCT Publication WO 2005/009453A1 discloses a process for the preparation of debitterised and
defatted fenugreek powder containing 4-hydroxy isoleucine and rich in soluble dietary fiber. The
process described includes extraction of powdered fenugreek seeds with ethanol/methanol to obtain
debitterised powder containing 4-hydroxy isoleucine. This debitterised powder on sieving through a
mesh size of 50 to 90 BSS yields upper and lower layers, of which upper layer is said to contain more
of soluble fiber about 40 to 45%. That the fenugreek seeds are treated in this process with polar
alcohols at elevated temperatures for debitterisation, the process may lead to loss of some amount of
dietary fibers. Further since the entire seed with the hus and embryo is utilized in this extraction
process, the debitterised powder obtained has higher protein content (20 - 45% by weight) which is
an undesirable attribute for a pharmaceutical or food excipient. PCT Publication WO.2009/057125A1
discloses a process for improving the organoleptic property of the dietary fiber obtained from the
seeds of fenugreek by debitterisation, deodourisation and decolonisation of the seed. The process
disclosed herein consist of the steps of soaking the plant parts overnight in a solvent; powdering plant
parts to obtain powder, extracting the powdered plant parts using a solvent; separating the extracted
components, precipitating the separated components to obtain gum; and washing precipitated gum
followed by drying to obtain organoleptically improved dietary fiber that comprises proteins around
25% and galactomannnans around 75%. Further since the entire seed is utilized in this extraction
process, dietary fiber obtained has high protein content which is an undesirable attribute for a
pharmaceutical or food excipient.
Thus methods disclosed in the art to isolate dietary fibers and other components from fenugreek seeds
are non-specific and involve the use of costly and specialized equipments, organic solvents or energy
intensive methods for extraction. Further the isolation of dietary fibers relates particularly to isolation
of soluble dietary fibers for their therapeutic use or to isolation of soluble fibers with high protein
content for nutritional purposes. Hence though attempts have been made towards isolating dietary
fibers primarily soluble fibers, these have not been directed to isolation of dietary fibers from
fenugreek having a particular ratio of insoluble to soluble fibers to obtain an excipient that can be
used in various pharmaceutical or cosmetic compositions and food, nutritional or dietary preparations.
Further various marketed products based on Fenugreek fibers available for health or nutritional
purposes also mainly have soluble fibers in their compositions with insoluble dietary fibers if present
being present at relatively low amounts. Fenfiber®, for example, manufactured by Emerald Seed
Products for blood sugar and cholesterol management as well as for good digestive health, comprises
92% total fiber content with 80% soluble and 12% insoluble fibers i.e., has ratio of insoluble to
soluble dietary fibers of 0.15. FenuPure from NatuR&D known to have properties of blocking the
adsorption of glucose into blood and binding cholesterol implicated in heart disease has a total fiber
content of greater than 85% and soluble fibers of greater than 80%, thereby having a ratio of insoluble
to soluble fibers of about 0.07. Thus particularly the art fails to teach isolation of dietary fibers from
fenugreek seeds comprising insoluble and soluble dietary fibers in a ratio of 0.2 to 1 and comprising
not more than 10 weight % of protein.
EP1697050 discloses solvent free process of obtaining insoluble fiber rich fraction and further a
highly purified fiber rich fraction from fenugreek seeds. The fractions obtained have at least 50% of
dietary fiber with ratio of insoluble to soluble dietary fiber of greater than 0.8, preferably greater than
1.2 and a protein content of not more than 10 weight %. Though the solvent free process provides
dietary fiber fractions with ratio of insoluble to soluble dietary fiber of greater than preferably .2, it
does not disclose in any manner dietary fiber fractions or processes for obtaining the same wherein
the ratio of insoluble to soluble fibers is lesser than and protein content not more than 10 weight %
that also exhibits necessary characteristics required of a pharmaceutical or food excipient such as
viscosity, swelling index, water holding capacity etc.
Varying ratios of insoluble and soluble fibers and other constituents such as proteins in the extracts
derived from fenugreek seeds determine the applicability of the extract as an excipient in
pharmaceutical or cosmetic compositions and food, nutritional or dietary preparations. Excipients
comprising insoluble and soluble fibers in a ratio of not more than ] have properties and applications
that are different from those comprising insoluble and soluble fibers in a ratio of more than 1. The
differences in the chemical constitution and thereby the properties of soluble and insoluble dietary
fibers results in differences in the applications of the products comprising them in varied ratios.
Additionally in cases where the ratio of insoluble to soluble dietary fibers is less than 1, fiber based
products with ratios of insoluble to soluble fibers of less than 0.2 do not possess properties desirable
of pharmaceutical excipient. The present inventors after identifying the importance of varied ratio of
insoluble to soluble fibers provide an excipient from fenugreek seeds comprising insoluble to soluble
dietary fibers in a ratio of less than 1 with protein content of not more than 0 weight % and
processes for production thereof. The excipient provided by the inventors of the present invention can
be used industrially as a pharmaceutical or food excipient.
SUMMARY OF THE INVENTION
The present invention relates to an excipient obtained from Trigonellafoenum-graceum seeds and a
process for preparation thereof. The invention further relates to an excipient obtained from Trigonella
foenum-graceum seeds, comprising not less than 50% dietary fibers with ratio of insoluble dietary
fibers to soluble dietary fibers of about 0.2 to about 1 and protein content of not more than about 10
weight%. The invention also relates to the use of this excipient in various pharmaceutical or cosmetic
compositions and food, nutritional or dietary preparations.
DETAILED DESCRIPTION OF THE INVENTION
The present invention provides an excipient obtained from Trigonella foenum-graceum comprising
dietary fibers in an amount of not less than 50% dietary fibers by weight of the excipient, wherein
said dietary fibers have a ratio of insoluble dietary fibers to soluble dietary fibers of about 0.2 to about
1; and protein content of not more than about 10 % by weight of the excipient. In one embodiment of
the present invention an excipient obtained from Trigonella foenum-graceum is disclosed that
comprises dietary fibers in an amount of not less than 50% by weight of the excipient, wherein said
dietary fibers have a ratio of insoluble dietary fibers to soluble dietary fibers of about 0.2 to about 0.8;
and protein content of not more than about 10 % by weight of the excipient. In a further embodiment
of the present invention an excipient obtained from Trigonella foenum-graceum is disclosed
comprising dietary fibers in an amount of not less than 50% by weight of the excipient, wherein said
dietary fibers have a ratio of insoluble dietary fibers to soluble dietary fibers of about 0.2 to about 0.7;
and protein content of not more than about 10 % by weight of the excipient. In a further embodiment
of the present invention an excipient obtained from Trigonella foenum-graceum is disclosed
comprising dietary fibers in an amount of not less than 50% by weight of the excipient, wherein said
dietary fibers have a ratio of insoluble dietary fibers to soluble dietary fibers of about 0.3 to about 0.8;
and protein content of not more than about 10 % by weight of the excipient. In a further embodiment
of the present invention an excipient obtained from Trigonella foenum-graceum is disclosed
comprising dietary fibers in an amount of not less than 50% by weight of the excipient, wherein
said dietary fibers have a ratio of insoluble dietary fibers to soluble dietary fibers of about 0.5 to about
0.8; and; protein content of not more than about 10 % by weight of the excipient.
In yet another aspect of the present invention is provided an excipient comprising dietary fibers in an
amount of about 50% to about 98% by weight of the excipient, wherein said dietary fibers have a
ratio of insoluble to soluble dietary fiber of about 0.2 to about 1; and protein content of not more than
10 weight %. In another embodiment is provided an excipient comprising dietary fibers in an amount
of about 50% to about 98% by weight the excipient, wherein said dietary fibers have a ratio of
insoluble to soluble dietary fiber of about 0.2 to about 0.8 and; protein content of not more than 10
weight %. In one embodiment is provided an excipient comprising dietary fibers in an amount of
about 50% to about 98% by weight the excipient, wherein said dietary fibers have a ratio of insoluble
to soluble dietary fiber of about 0.2 to about 0.7 and; protein content of not more than 10 weight %. In
a further embodiment is provided an excipient comprising dietary fibers in an amount of about 50%
to about 98% by weight the excipient, wherein said dietary fibers have a ratio of insoluble to soluble
dietary fiber of about 0.3 to about 0.8 and; protein content of not more than 10 weight %.In a still
another embodiment of the present invention is provided an excipient obtained from Trigonella
foenum-graceum comprising dietary fibers in an amount of not less than 50% by weight of the
excipient, wherein said dietary fibers have a ratio of insoluble dietary fibers to soluble dietary fibers
of about 0.2 to about 1 and protein content of not more than about 10 weight % having a viscosity
greater than 10000 cps at 2% w/v concentration at 25°C. In another embodiment of the present
invention is provided an excipient obtained from Trigonella foenum-graceum comprising not less
than 50% dietary fibers with ratio of insoluble dietary fibers to soluble dietary fibers of about 0.2 to
about 0.8 and protein content of not more than about 10 weight % having a viscosity greater than
10000 cps at 2% w/v concentration at 25°C. In a further embodiment of the present invention is
provided an excipient obtained from Trigonella foenum-graceum comprising not less than 50%
dietary fibers with ratio of insoluble dietary fibers to soluble dietary fibers of about 0.2 to about 0.7
and protein content of not more than about 0 weight % having a viscosity greater than 10000 cps at
2% w/v concentration at 25°C. n a one embodiment of the present invention is provided an excipient
obtained from Trigonellafoenum-graceum comprising not less than 50% dietary fibers with ratio of
insoluble dietary fibers to soluble dietary fibers of about 0.3 to about 0.8 and protein content of not
more than about 0 weight % having a viscosity greater than 10000 cps at 2% w/v concentration at
25°C. In a still another embodiment of the present invention is provided an excipient obtained from
Trigonella foenum-graceum comprising not less than 50% dietary fibers with ratio of insoluble
dietary fibers to soluble dietary fibers of about 0.2 to about 1 and protein content of not more than
about 10 weight % having a swelling index greater than about 6 ml/g of excipient. In another
embodiment of the present invention is provided an excipient obtained from Trigonella foenumgraceum
comprising not less than 50% dietary fibers with ratio of insoluble dietary fibers to soluble
dietary fibers of about 0.2 to about 1 and protein content of not more than about 10 weight % having a
swelling index of about 6 ml/g of excipient to about 40ml/g of excipient. In a still another
embodiment of the present invention is provided an excipient obtained from Trigonella foenumgraceum
comprising not less than 50% dietary fibers with ratio of insoluble dietary fibers to soluble
dietary fibers of about 0.2 to about 0.8 and protein content of not more than about 10 weight %
having a swelling index greater than about 6 ml/g of excipient. In a further embodiment of the present
invention is provided an excipient obtained from Trigonella foenum-graceum comprising not less
than 50% dietary fibers with ratio.of insoluble dietary fibers to soluble dietary fibers of about 0.2 to
about 0.7 and protein content of not more than about 10 weight % having a swelling index greater
than about 6 ml/g of excipient. In another embodiment of the present invention is provided an
excipient obtained from Trigonellafoenum-graceum comprising not less than 50% dietary fibers with
ratio of insoluble dietary fibers to soluble dietary fibers of about 0.3 to about 0.8 and protein content
of not more than about 10 weight % having a swelling index greater than about 6 ml/g of excipient. In
another embodiment of the present invention is provided an excipient obtained from Trigonella
foenum-graceum comprising not less than 50% dietary fibers with ratio of insoluble dietary fibers to
soluble dietary fibers of about 0.2 to about 1 and protein content of not more than about 0 weight %
having a swelling index greater than about 15 ml/g of excipient. In one embodiment of the present
invention is provided an excipient obtained from Trigonella foenum-graceum comprising not less
than 50% dietary fibers with ratio of insoluble dietary fibers to soluble dietary fibers of about 0.2 to
about 1 and protein content of not more than about 10 weight % having a swelling index of about 5
ml/g of excipient to about 40ml/g of excipient. In one embodiment of the present invention is
provided an excipient obtained from Trigonella foenum-graceum comprising not less than 50%
dietary fibers with ratio of insoluble dietary fibers to soluble dietary fibers of about 0.2 to about 0.8
and protein content of not more than about 10 weight % having a swelling index greater than about 5
ml/g of excipient. In a further embodiment of the present invention is provided an excipient obtained
from Trigonellafoenum-graceum comprising not less than 50% dietary fibers with ratio of insoluble
dietary fibers to soluble dietary fibers of about 0.2 to about 0.7 and protein content of not more than
about 10 weight % having a swelling index greater than about 15 ml/g of excipient. In another
embodiment of the present invention is provided an excipient obtained from Trigonella foenumgraceum
comprising not less than 50% dietary fibers with ratio of insoluble dietary fibers to soluble
dietary fibers of about 0.3 to about 0.8 and protein content of not more than about 10 weight %
having a swelling index greater than about 15 ml/g of excipient. In a still another embodiment of the
present invention is provided an excipient obtained from Trigonellafoenum-graceum comprising not
less than 50% dietary fibers with ratio of insoluble dietary fibers to soluble dietary fibers of about 0.2
to about 1 and protein content of not more than about 10 weight % having a water holding capacity
greater than about 8 g of water/g of excipient. In another embodiment of the present invention is
provided an excipient obtained from Trigonella foenum-graceum comprising not less than 50%
dietary fibers with ratio of insoluble dietary fibers to soluble dietary fibers of about 0.2 to about 1 and
protein content of not more than about 0 weight % having a water holding capacity of about 8 g of
water/g of excipient to about 50 g of water/g of excipient. In one embodiment of the present invention
is provided an excipient obtained from Trigonella foenum-graceum comprising not less than 50%
dietary fibers with ratio of insoluble dietary fibers to soluble dietary fibers of about 0.2 to about 0.8
and protein content of not more than about 0 weight % having a water holding capacity greater than
about 8 g of water/g of excipient. In another embodiment of the present invention is provided an
excipient obtained from Trigonellafoenum-graceum comprising not less than 50% dietary fibers with
ratio of insoluble dietary fibers to soluble dietary fibers of about 0.2 to about 0.7 and protein content
of not more than about 10 weight % having a water holding capacity greater than about 8 g of water/g
of excipient. In a still another embodiment of the present invention is provided an excipient obtained
from Trigonellafoenum-graceum comprising not less than 50% dietary fibers with ratio of insoluble
dietary fibers to soluble dietary fibers of about 0.3 to about 0.8 and protein content of not more than
about 10 weight % having a water holding capacity greater than about 8 g of water/g of excipient. In
another embodiment of the present invention is provided an excipient obtained from Trigonella
foenum-graceum comprising not less than 50% dietary fibers with ratio of insoluble dietary fibers to
soluble dietary fibers of about 0.2 to about 1 and protein content of not more than about 10 weight %
having a water holding capacity greater than about 20 g of water/g of excipient. In one embodiment
of the present invention is provided an excipient obtained from Trigonella foenum-graceum
comprising not less than 50% dietary fibers with ratio of insoluble dietary fibers to soluble dietary
fibers of about 0.2 to about 1 and protein content of not more than about 10 weight % having a water
holding capacity of about 20 g of water/g of excipient to about 50 g of water/g of excipient. n one
embodiment of the present invention is provided an excipient obtained from Trigonella foenumgraceum
comprising not less than 50% dietary fibers with ratio of insoluble dietary fibers to soluble
dietary fibers of about 0.2 to about 0.8 and protein content of not more than about 10 weight %
having a water holding capacity greater than about 20 g of water/g of excipient. n another
embodiment of the present invention is provided an excipient obtained from Trigonella foenumgraceum
comprising not less than 50% dietary fibers with ratio of insoluble dietary fibers to soluble
dietary fibers of about 0.2 to about 0.7 and protein content of not more than about 10 weight %
having a water holding capacity greater than about 20 g of water/g of excipient. In still another
embodiment of the present invention is provided an excipient obtained from Trigonella foenumgraceutn
comprising not less than 50% dietary fibers with ratio of insoluble dietary fibers to soluble
dietary fibers of about 0.3 to about 0.8 and protein content of not more than about 10 weight %
having a water holding capacity greater than about 20 g of water/g of excipient. In one aspect,
viscosity, swel ling index and water holding capacity are analyzed as per non-limiting illustrative
examples discussed.
In a further embodiment of the present invention is provided an excipient comprising dietary fibers in
an amount of not less than 50% dietary fibers by weight of the excipient, wherein said dietary fibers
have a ratio of insoluble dietary fibers to soluble dietary fibers of about 0.2 to about 1; and protein
content of not more than about 0 % by weight of the excipient; wherein the excipient is further
characterized by being substantially free of 4-hydroxyisoleucine. In one embodiment of the present
invention is provided an excipient comprising dietary fibers in an amount of not less than 5 0% dietary
fibers by weight of the excipient, wherein said dietary fibers have a ratio of insoluble dietary fibers to
soluble dietaiy fibers of about 0.2 to about 0.8; and protein content of not more than about 0 % by
weight of the excipient; wherein the excipient is further characterized by being substantially free of 4-
hydroxyisoleucine. n a further embodiment of the present invention is provided an excipient
comprising dietary fibers in an amount of not less than 50% dietary fibers wherein said dietary fibers
have a ratio of insoluble dietary fibers to soluble dietary fibers of about 0.2 to about 1; and protein
content of not more than about 10 % by weight of the excipient; wherein the excipient is further
characterized by being substantially free of saponins. n one embodiment of the present invention is
provided an excipient comprising dietary fibers in an amount of not less than 50% dietary fibers
wherein said dietary fibers have a ratio of insoluble dietary fibers to soluble dietary fibers of about 0.2
to about 0.8; and protein content of not more than about 0 % by weight of the excipient; wherein the
excipient is further characterized by being substantially free of saponins. In a further embodiment of
the present invention is provided an excipient comprising dietary fibers in an amount of not less than
50% dietary fibers wherein said dietary fibers have a ratio of insoluble dietary fibers to soluble
dietary fibers of about 0.2 to about 1; and protein content of not more than about 0 % by weight of
the excipient; wherein the excipient is further characterized by being substantially free of alkaloids. In
one embodiment of the present invention is provided an excipient comprising dietary fibers in an
amount of not less than 50% dietary fibers wherein said dietary fibers have a ratio of insoluble dietary
fibers to soluble dietary fibers of about 0.2 to about 0.8; and protein content of not more than about 10
% by weight of the excipient; wherein the excipient is further characterized by being substantially
free of alkaloids, in another embodiment of the present invention is provided an excipient comprising
dietary fibers in an amount of not less than 50% dietary fibers wherein said dietary fibers have a ratio
of insoluble dietaty fibers to soluble dietary fibers of about 0.2 to about 1; and protein content of not
more than about 0 % by weight of the excipient; wherein the excipient is further characterized by
being substantially free of 4-hydroxyisoleucine, alkaloids, saponins or sapogenins. In one
embodiment of the present invention is provided an excipient comprising dietary fibers in an amount
of not less than 50% dietary fibers wherein said dietary fibers have a ratio of insoluble dietary fibers
to soluble dietary fibers of about 0.2 to about 0.8; and protein content of not more than about 10 % by
weight of the excipient; wherein the excipient is further characterized by being substantially free of 4-
hydroxyisoleucine, alkaloids, saponins or sapogenins. In another embodiment of the present invention
is provided an excipient comprising dietary fibers in an amount of not less than 50% dietary fibers
wherein said dietary fibers have a ratio of insoluble dietary fibers to soluble dietary fibers of about 0.2
to about ; and protein content of not more than about 10 % by weight of the excipient; wherein the
excipient is further characterized by being substantially free of 4-hydroxyisoleucine, alkaloids,
saponins and sapogenins. In another embodiment of the present invention is provided an excipient
comprising dietary fibers in an amount of not less than 50% dietary fibers wherein said dietary fibers
have a ratio of insoluble dietary fibers to soluble dietary fibers of about 0.2 to about 0.8; and protein
content of not more than about 10 % by weight of the excipient; wherein the excipient is further
characterized by being substantially free of 4-hydroxyisoleucine, alkaloids, saponins and sapogenins.
In one embodiment, the term "substantially free" as used herein means the excipient of the present
invention obtained from Trigonellafoenum-graceum may comprise not more than 1% by weight of 4-
hydroxyisoleucine. In another embodiment, the term "substantially free" as used herein means the
excipient of the present invention obtained from Trigonellafoenum-graceum may comprise not more
than 0.4% of 4-hydroxyisoleucine. In one embodiment, the term "substantially free" as used herein
means the excipient of the present invention obtained from Trigonella foenum-graceum may
comprise not more than 0.2% of 4-hydroxyisoleucine. In another embodiment, the term
"substantially free" as used herein means the excipient of the present invention obtained from
Trigonellafoenum-graceum may comprise not more than 5% of alkaloids such as, but not limited to,
trigonelline, gentianine, carpaine or choline and the like. n a further embodiment, the term
"substantially free" as used herein means the excipient of the present invention obtained from
Trigonellafoenum-graceum may comprise not more than 1% of alkaloids such as, but not limited to,
trigonelline, gentianine, carpaine or choline and the like. In another embodiment, the term
"substantially free" as used herein means the excipient of the present invention obtained from
Trigomlla foenum-graceum may comprise not more than 0.5% of alkaloids such as, but not limited
to, trigonelline, gentianine, carpaine or choline and the like. In a further embodiment, the term
"substantially free" as used herein means the excipient of the present invention obtained from
Trigonellafoenum-graceum may comprise not more than 0.1% of alkaloids such as, but not limited
to, trigonelline, gentianine, carpaine or choline and the like. In a further embodiment, the term
"substantially free" as used herein means the excipient of the present invention obtained from
Trigonellafoenum-graceum may comprise not more than 5% of saponins such as, but not limited to,
trigonelloside C, trigofoenoside A, trigofoenoside B, trigofoenoside C, trigofoenoside D,
trigofoenoside E, trigofoenoside F, trigofoenoside G, trigoneosides la, trigoneoside b, trigoneoside
Ila, trigoneoside b, trigoneoside Ilia, trigoneoside Illb, neogitogenin, trigoneoside IX, trigoneoside
Xa, trigoneoside Xb, trigoneoside Xlb, trigoneoside Xlla, trigoneoside Xllb, trigoneoside X a,
graecunin H, graecunin I, graecunin J, graecunin K, graecunin L, graecunin , graecunin N, fenugrin
B . In a further embodiment, the term "substantially free" as used herein means the excipient of the
present invention obtained from Trigonella foenum-graceum may comprise not more than 1% of
saponins such as, but not limited to, trigonelloside C, trigofoenoside A, trigofoenoside B,
trigofoenoside C, trigofoenoside D, trigofoenoside E, trigofoenoside F, trigofoenoside G,
trigoneosides la, trigoneoside lb, trigoneoside Ila, trigoneoside lib, trigoneoside la, trigoneoside
Illb, neogitogenin, trigoneoside IX, trigoneoside Xa, trigoneoside Xb, trigoneoside Xlb, trigoneoside
Xlla, trigoneoside Xllb, trigoneoside X a, graecunin H, graecunin I, graecunin J, graecunin K,
graecunin L, graecunin M, graecunin N, fenugrin B. In a further embodiment, the term "substantially
free" as used herein means the excipient of the present invention obtained from Trigonellafoenumgraceum
may comprise not more than 0.5% of saponins such as, but not limited to, trigonelloside C,
trigofoenoside A, trigofoenoside B, trigofoenoside C, trigofoenoside D, trigofoenoside E,
trigofoenoside F, trigofoenoside G, trigoneosides la, trigoneoside lb, trigoneoside Ila, trigoneoside
b, trigoneoside Ilia, trigoneoside Illb, neogitogenin, trigoneoside IX, trigoneoside Xa, trigoneoside
Xb, trigoneoside Xlb, trigoneoside Xlla, trigoneoside X b, trigoneoside Xllla, graecunin H,
graecunin I, graecunin J, graecunin K, graecunin L, graecunin M, graecunin N, fenugrin B. In a
further embodiment, the term "substantially free" as used herein means the excipient of the present
invention obtained from Trigonellafoenum-graceum may comprise not more than 0.1% of saponins
such as, but not limited to, trigonelloside C, trigofoenoside A, trigofoenoside B, trigofoenoside C,
trigofoenoside D, trigofoenoside E, trigofoenoside F, trigofoenoside G, trigoneosides la, trigoneoside
lb, trigoneoside a, trigoneoside lib, trigoneoside Ilia, trigoneoside lllb, neogitogenin, trigoneoside
IX, trigoneoside Xa, trigoneoside Xb, trigoneoside Xlb, trigoneoside X a, trigoneoside Xllb,
trigoneoside Xllla, graecunin H, graecunin I, graecunin J, graecunin , graecunin L, graecunin M,
graecunin N, fenugrin B. In a further embodiment, the term "substantially free" as used herein means
the excipient of the present invention obtained from Trigonella foenum-graceum may comprise not
more than 5% of sapogenins such as, but not limited to, diosgenin, yamogenin, yuccagenin, lilagenin,
tigogenin, neotigogenin, gitogenin, neogitogenin, smilagenin, sarsapogenin. In a further embodiment,
the term "substantially free" as used herein means the excipient of the present invention obtained
from Trigonella foenum-graceum may comprise not more than % of sapogenins such as, but not
limited to, diosgenin, yamogenin, yuccagenin, lilagenin, tigogenin, neotigogenin, gitogenin,
neogitogenin, smilagenin, sarsapogenin. In a further embodiment, the term "substantially free" as
used herein means the excipient of the present invention obtained from Trigonellafoenum-graceum
may comprise not more than 0.5% of sapogenins such as, but not limited to, diosgenin, yamogenin,
yuccagenin, lilagenin, tigogenin, neotigogenin, gitogenin, neogitogenin, smilagenin, sarsapogenin. n
a further embodiment, the term "substantially free" as used herein means the excipient of the present
invention obtained from Trigonella foenum-graceum may comprise not more than 0.1% of
sapogenins such as, but not limited to, diosgenin, yamogenin, yuccagenin, lilagenin, tigogenin,
neotigogenin, gitogenin, neogitogenin, smilagenin, sarsapogenin.
In a further aspect the present invention provides process for obtaining an excipient, comprising not
less than 50% dietary fibers with ratio of insoluble dietary fibers to soluble dietary fibers of about 0.2
to about 1 and protein content of not more than about 0 weight%. The process of the present
invention utilizes equipments commonly employed in the pharmaceutical industry thereby
simplifying scale-up and commercialization in comparison with prior art processes using specialized
equipments.
The process steps involved in the preparation of excipient of the present invention from Trigonella
foenuin-graceum seeds have been discussed in further details beneath. Any modifications of the
process steps apparent to a person skilled in the art are encompassed within the scope of the present
invention.
( ) Selection of Trigonella foenum-graecum seeds of predetermined dimensions and swelling factor:
Seeds having length between 3.0-6.0 mm, preferably 3.5-4.5mm and breadth ranging from 1.5-4.0
mm, preferably 2.0-3.5 mm are selected. Seeds with swelling factor ranging 0.5-50.0 ml, preferably
3.0-35.0 ml are used in the isolation process. Moisture content of the fenugreek seeds is also
determined. Seeds with a moisture content of greater than 10% are difficult to process. In such cases
the seeds are dried at 60°C to achieve the moisture level of less than 10% and then subsequently
employed for isolation of the excipient of the present invention.
(2) Roasting the selected seeds:
Seeds of Trigonella foenum-graecum are roasted to facilitate separation of embryo and husk. This
step is carried out using a flaking drum or any other suitable equipment wherein seeds are roasted in a
rotating drum at temperature >50°C whereby the bond between the husk and embryo is loosened.
(3) Subjecting the seeds/roasted seeds to differential milling to obtain a mixture of embryo and husk
The selected seeds roasted or non-roasted are milled to isolate the husk. The physical treatment
process entails milling the selected roasted or non-roasted Trigonella foenum-graceum seeds in an
impact three roller mill. Any mill such as, but not limited to comminuting mill, hammer mill, which is
able to mill-break the Trigonellafoenum-graceum seeds can be employed. Fenugreek seed is known
to have central, hard yellow embryo, which is surrounded by husk comprising of corneous endosperm
and tenacious testa. The differential milling operation results in physical separation of husk from the
yellow embryo, to make a mixture of the two components physically together, but no longer
physically attached to each other, n the differential milling process the embryo is milled due to its
rigid nature and the husk being fibrous is not pulverized. n one embodiment the husk is further
processed to separate the testa and the endosperm which can be blended in different proportions.
(4) Separation of husk from embryo
Separation of husk and the yellow embryo from the physical blend obtained after milling may be
carried out by sieving through any sieve greater than 8#. The fraction passing through the sieve i.e.,
the yellow embryo-rich fraction is discarded and the fraction retained on the sieve is the fraction rich
in husk. When employing roasted seeds, the husk fraction obtained after milling contains not more
than 20% of embryo, preferably not more than 10% of embryo, more preferably not more than 5% of
embryo. The husk fraction obtained after milling when non-roasted seeds are employed may still
contain about 20% of the yellow embryo and further separation of this is carried out by a process
based on the density difference between the husk and the yellow embryo. n another embodiment, the
process of further separation of husk and embryo based on differential density between the two
involves fluidization of the physical blend of fraction rich in husk and yellow embryo in a stream of
air. As yellow embryo is denser than husk fraction, the husk is blown away during fluidization in a
separate chamber whereas the yellow embryo remains in the same chamber. The husk-containing
fraction is further sieved through 8# to obtain a husk rich excipient. The embryo content in husk-rich
fraction is less than 20%, preferably less than 10%, preferably less than 5%.
(5) Sizing the separated husk to desired particle size:
The separated husk rich fraction is further milled using a roller mill, grinding mill or any other
suitable mill to the desired particle size. This sized separated husk can be employed as excipient of
the present invention that has unique properties resulting from the combination of soluble as well as
insoluble dietary fiber.
(6) Tempering/hydrating the separated husk/separated sized husk/husk:
Tempering/hydrating the separated husk or separated sized husk or husk with deminerahsed water
helps in sizing the fibrous husk to desired particle size distribution. Hydration is carried out using
about 50% to about 200% deminerahsed water.
(7) Compaction and drying of the hydrated husk and sizing the compacted mass
Compaction of hydrated husk followed by drying and sizing also helps in sizing the fibrous husk to
desired particle size distribution. Compaction of hydrated husk is carried out using flat rolls or any
other suitable equipment known to a person skilled in the art. The compacted mass is dried using
dryer to loss on drying of less than about 2%. Sizing of the compacted mass may be carried out by
milling to obtain excipient of the present invention with desired particle size distribution and
comprising not less than 50% dietary fibers with ratio of insoluble dietary fibers to soluble dietary
fibers of about 0.2 to 1 and protein content of not more than 10 weight%.
(8) Purification of dietary fibers
The first step is preparation of dispersion of from about 0.1- 10% w/v of sized husk/separated sized
husk/separated husk/husk in a solvent. The process is carried out at room temperature and ambient
atmospheric pressure; however, higher temperatures can be employed if necessary. Solvent used for
extraction may be selected from water, acidified water or any other solvent in which the sized husk
can produce dispersion. In one embodiment acetic acid is used for extraction as it results in increased
yield and whiter product. The concentration of sized husk is only limited by the processibility as at
higher concentrations due to increased viscosity stirring becomes difficult. The dispersion is then
filtered or centrifuged. The insoluble fraction is subjected to further extraction using a solvent for
better recovery.
The filtered dispersion is treated with an appropriate volume of a water-miscible, pharmaceutically
acceptable solvent, which causes the precipitation of dietary fibers. Any of the pharmaceutically
acceptable lower alkyl alcohols or ketones such as ethanol, methanol, isopropyl alcohol, acetone, and
the like is suitable for precipitation and can be employed. In one embodiment methanol is used as a
solvent. The ratio of the volumes of the water-miscible solvent to the dispersion may vary from about
1 to 5 to 5 to 1. To minimize the volume of solvent used, the volume of the dispersion may be
reduced by evaporating water before adding the solvent. The resulting hairy fibers are separated from
the liquids by any means known to one skilled in the art such as centrifugation or filtration.
(9) Washing the precipitate, followed by filtering, drying and sizing:
Further purification of the white hairy fibers is carried out using any of the pharmaceutically
acceptable lower alkyl alcohols or ketones, such as, but not limited to, ethanol, isopropyl alcohol,
acetone, and the like. This step removes the traces of moisture present in the fibrous precipitate and
thereby aids in dry ing of the product at lower temperature conditions. The resulting excipient is dried
at a temperature less than 100°C for a period of time sufficient to dry the material to moisture content
of less than 10%. Drying can be carried out using any of the equipments such as tray dryer, fluidized
bed dryer, vacuum dryer etc. The conditions for drying are however very critical as high temperature,
humidity and the rate of drying may cause discoloration of the product. Once the dried material is
obtained it is further broken up to a suitable particle size by any means known in the art to obtain
excipient of the present invention comprising not less than 50% dietary fibers with ratio of insoluble
dietary fibers to soluble dietary fibers of about 0.2 to and protein content of not more than 0
weight%.
(10) Spray-drying
Than washing the precipitated fibers, followed by filtering, drying and sizing, the separated purified
dietary fibers of (8) above are alternatively resuspended and spray dried. Spray drying is an industrial
process involving particle formation and drying. It is highly suited for the continuous production of
dry solids in either powder, granulate or agglomerate form from liquid feedstock such as solutions,
emulsions and pumpable suspensions. Spray drying involves the atomization of a liquid feedstock
into a spray of droplets that are contacted with hot air in a drying chamber. The sprays are produced
by rotary (wheel), nozzle, or ultrasonic atomizers. Evaporation of moisture from the droplets as the
dry particles are formed proceeds under controlled temperature and airflow conditions. The dry
product is discharged continuously from the drying chamber. Operating conditions and dryer design
are selected according to the drying characteristics of the desired product, as is known in the art.
There are a number of variables in the spray drying process, including feed composition, feed
viscosity, density, feed spray rate, inlet temperature, outlet temperature, temperature difference,
atomization pressure, vacuum and residence time, which can be varied in order to achieve the desired
product. An illustrative process employed to produce the excipient of the present invention comprises
dissolving/suspending the purified dietary fibers by homogenization in a suitable aqueous solvent,
typically water or water miscible solvents to form slurry. The slurry may be preheated under stirring
before being fed into the spray drying chamber, and may be sprayed with a single fluid nozzle or a
two-fluid nozzle. Alternatively, the slurry may be sprayed using a rotating disk. The drying of the
particles is achieved using any of the methods such as co-current flow, counter current flow or mixed
flow. The total solid content of the feed could vary from about 0.05-75%.
Further some non-limiting embodiments describing the process employed to obtain excipient of the
present invention comprising not less than 50% dietary fibers with ratio of insoluble dietary fibers to
soluble dietary fibers of about 0.2 to about 1 and protein content of not more than about 10 weight%
are discussed beneath.
In one embodiment a process for preparation of excipient of the present invention comprises a)
selecting Trigonella foenum-graecum seeds of predetermined dimensions and swelling factor; b)
roasting the seeds to facilitate separation of embryo and husk; c) subjecting the roasted seeds to
differential milling to obtain a mixture of embryo and husk in which the embryo breaks in the form of
particles; d) passing a mixture through a sieve to substantially separate the embryo and the husk to
obtain husk fraction containing not more than 20% of embryo, preferably not more than 10% of
embryo, more preferably not more than 5% of embryo; e) sizing of the separated husk to obtain
excipient of the present invention comprising not less than 50% dietary fibers with ratio of insoluble
dietary fibers to soluble dietary fibers of about 0.2 to 1 and protein content of not more than 10
weight%.
Another embodiment relates to a process for preparation of excipient of the present invention
comprising a) selecting Trigomlla foenum-graecum seeds of predetermined dimensions and swelling
factor; b) roasting the seeds to facilitate separation of embryo and husk; c) subjecting the roasted
seeds to differential milling to obtain a mixture of embryo and husk in which the embryo breaks in
the form of particles; d) passing a mixture through a sieve to substantially separate the embryo and
the husk to obtain husk fraction containing not more than 20% of embryo, preferably not more than
10% of embryo, more preferably not more than 5% of embryo; e) sizing of the separated husk; f
tempering/hydrating the sized husk with demineralised water; g) compacting and drying the mass; h)
sizing the compacted mass to obtain excipient of the present invention comprising not less than 50%
dietary fibers with ratio of insoluble dietary fibers to soluble dietary fibers of about 0.2 to 1 and
protein content of not more than 0 weight%.
A still another embodiment relates to a process for preparation of excipient of the present invention
comprising a) selecting Trigonellafoenum-graecum seeds of predetermined dimensions and swelling
factor; b) subjecting the seeds to differential milling to obtain a mixture of embryo and husk in which
the embryo breaks in the form of particles; c) passing a mixture through a sieve to substantially
separate the embryo and the husk, the separated husk fraction containing not more than 20% of
embryo; d) separation of the husk from any embryo remnants based on density difference between
them to provide separated husk containing preferably not more than 10% of embryo, more preferably
not more than 5% of embryo; e) sizing of the separated husk; f ) tempering/hydrating the sized husk
with demineralised water; g) compacting and drying the mass; h) sizing the compacted mass to obtain
excipient of the present invention comprising not less than 50% dietary fibers with ratio of insoluble
dietary fibers to soluble dietary fibers of about 0.2 to 1 and protein content of not more than 0
weight%.
Another embodiment relates to a process for preparation of excipient of the present invention
comprising a) selecting Trigonellafoenum-graecum seeds of predetermined dimensions and swelling
factor; b) subjecting the seeds to differential milling to obtain a mixture of embryo and husk in which
the embryo breaks in the form of particles; c) passing a mixture through a sieve to substantially
separate the embryo and the husk, the separated husk fraction containing not more than 20% of
embryo; d) separation of the husk from any embryo remnants based on density difference between
t em to provide separated husk containing preferably not more than 0% of embryo, more preferably
not more than 5% of embryo; e) sizing of the separated husk; f) analyzing the sized husk for its
endosperm content or water holding capacity or swelling index or viscosity; g) selecting husk with an
endosperm content of not less than 15% or a water holding capacity of not less than 6 g of water per g
of husk or a swelling index of not less than 5 ml per g of husk or a viscosity of not less than 500 cps
of 1% w/v solution; h) tempering/hydrating the selected sized husk with demineralised water; i)
compacting and drying the mass; j ) sizing the compacted mass to obtain excipient of present
invention comprising not less than 50% dietary fibers with ratio of insoluble dietary fibers to soluble
dietary fibers of about 0.2 to 1 and protein content of not more than 0 weight%.
Yet another embodiment relates to a process for preparation of excipient of the present invention
comprising a) selecting Trigonellafoenum-graecum seeds of predetermined dimensions and swelling
factor; b) roasting the seeds to facilitate separation of embryo and husk; c) subjecting the roasted
seeds to differential milling to obtain a mixture of embryo and husk in which the embryo breaks in
the form of particles; d) passing a mixture through a sieve to substantially separate the embryo and
the husk to obtain husk fraction containing not more than 20% of embryo, preferably not more than
10% of embryo, more preferably not more than 5% of embryo; e) sizing of the separated husk; f )
preparing a 2% w/v dispersion of sized husk in acidified water and sieving it to obtain translucent
dispersion; g) precipitating fibers from translucent dispersion with polar alcohol; h) washing
precipitate with solvents; i) filtering and drying; j ) powdering to desired particle size to obtain
excipient of the present invention comprising not less than 50% dietary fibers with ratio of insoluble
dietary fibers to soluble dietary fibers of about 0.2 to 1 and protein content of not more than 0
weight%.
Another embodiment relates to a process for preparation of excipient of the present invention
comprising a) selecting Trigonellafoenum-graecum seeds of predetermined dimensions and swelling
factor; b) subjecting the seeds to differential milling to obtain a mixture of embryo and husk in which
the embryo breaks in the form of particles; c) passing a mixture through a sieve to substantially
separate the embryo and the husk, the separated husk fraction contains some embryo portion; d)
subjecting the separated husk again to milling and separation so as to obtain husk fraction containing
not more than 20% of embryo; e) separation of the husk from any embryo remnants based on density
difference between them to provide separated husk containing preferably not more than 10% of
embryo, more preferably not more than 5% of embryo; f) sizing of the separated husk; g) preparing a
2% w/v dispersion of sized husk in acidified water and sieving it to obtain translucent dispersion; h)
precipitating fibers from translucent dispersion with polar alcohol; i) washing precipitate with
solvents; j ) filtering and drying; k) powdering to desired particle size to obtain excipient of the
present invention comprising not less than 50% dietary fibers with ratio of insoluble dietary fibers to
soluble dietary fibers of about 0.2 to 1 and protein content of not more than 0 weight%.
Yet another embodiment relates to a process for preparation of excipient of the present invention
comprising a) selecting Trigonellafoenum-graecum seeds of predetermined dimensions and swelling
factor; b) roasting the seeds to facilitate separation of embryo and husk; c) subjecting the roasted
seeds to differential milling to obtain a mixture of embryo and husk in which the embryo breaks in
the form of particles; d) passing a mixture through a sieve to substantially separate the embryo and
the husk to obtain husk fraction containing not more than 20% of embryo, preferably not more than
10% of embryo, more preferably not more than 5% of embryo; e) sizing of the separated husk; )
preparing a 2% w/v dispersion of sized husk in acidified water and sieving it to obtain translucent
dispersion; g) precipitating fibers from translucent dispersion with polar alcohol; h) resuspending the
precipitated fibers by homogenization followed by spray drying to obtain excipient of the present
invention comprising not less than 50% dietary fibers with ratio of insoluble dietary fibers to soluble
dietary fibers of about 0.2 to 1 and protein content of not more than 10 weight.%.
Another embodiment relates to a process for preparation of excipient of the present invention
comprising a) selecting Trigonellafoenum-graecum seeds of predetermined dimensions and swelling
factor; b) subjecting the seeds to differential milling to obtain a mixture of embryo and husk in which
the embryo breaks in the form of particles; c) passing a mixture through a sieve to substantially
separate the embryo and the husk, the separated husk fraction contains some embryo portion; d)
subjecting the separated husk again to milling and separation so as to obtain husk fraction containing
not more than 20% of embryo; e) separation of the husk from any embryo remnants based on density
difference between them to provide separated husk containing preferably not more than 10% of
embryo, more preferably not more than 5% of embryo; f) sizing of the separated husk; g) preparing a
2% w/v dispersion of sized husk in acidified water and sieving it to obtain translucent dispersion; h)
precipitating fibers from translucent dispersion with polar alcohol; i) resuspending the precipitated
fibers by homogenization followed by spray drying to obtain excipient of the present invention
comprising not less than 50% dietary fibers with ratio of insoluble dietary fibers to soluble dietary
fibers of about 0.2 to 1 and protein content of not more than 0 weight%.
n a further embodiment in order to prepare the excipient of the present invention with desired
properties the separated husk or separated sized husk or husk may be selected with an endosperm
content of not less than % or a water holding capacity of not less than 6 g of water per gram of
material or a swelling index of not less than 5 ml per g of material or a viscosity of not less than 500
cps of l%w/v solution. n another embodiment of the present invention the separated husk or
separated sized husk or husk may be selected with an endosperm content of not less than 20% or a
water holding capacity of not less than 6 g of water per gram of material or a swelling index of not
less than 5 ml per g of material or a viscosity of not less than 500 cps of l%w/v solution. In still
another embodiment of the present invention the separated husk or separated sized husk or husk may
be selected with an endosperm content of not less than 15% or a water holding capacity of not less
than 6 g of water per gram of material or a swelling index of not less than 5 ml per g of material or a
viscosity of not less than 2000 cps of l%w/v solution. Selection of husk with the above parameters
aids obtain excipient of the present invention with desired properties.
n one embodiment, the process for preparation of an excipient from Trigonella foenum-gracewn
seeds as per the present invention comprises: a) selecting Trigonella foenum-graecum seeds of
predetermined dimensions and swelling factor; b) roasting the seeds to facilitate separation of embryo
and husk; c) subjecting the roasted seeds to differential milling to obtain a mixture of embryo and
husk in which the embryo breaks in the form of particles; d) passing a mixture through a sieve to
substantially separate the embryo and the husk to obtain separated husk fraction containing not more
than 20% of embryo; and e) sizing of the separated husk.
In another embodiment, the process for preparation of an excipient from Trigonellafoenum-graceum
seeds as per the present invention comprises: a) selecting Trigonella foenum-graecum seeds of
predetermined dimensions and swelling factor; b) roasting the seeds to facilitate separation of embryo
and husk; c) subjecting the roasted seeds to differential milling to obtain a mixture of embryo and
husk in which the embryo breaks in the form of particles; d) passing a mixture through a sieve to
substantially separate the embryo and the husk to obtain separated husk fraction containing not more
than 20% of embryo; e) sizing of the separated husk; f) preparing a dispersion of sized separated husk
in acidified water and sieving it to obtain translucent dispersion; g) precipitating fibers from
translucent dispersion with polar alcohol; h) washing precipitate with solvents; i) filtering and drying;
and j ) powdering to desired particle size.
In one embodiment, the process for preparation of an excipient from Trigonella foenum-graceum
seeds as per the present invention comprises: a) selecting Trigonella foenum-graecum seeds of
predetermined dimensions and swelling factor; b) roasting the seeds to facilitate separation of embryo
and husk; c) subjecting the roasted seeds to differential milling to obtain a mixture of embryo and
husk in which the embryo breaks in the form of particles; d) passing a mixture through a sieve to
substantially separate the embryo and the husk to obtain separated husk fraction containing not more
than 20% of embryo; and e) sizing of the separated husk; f tempering/hydrating the sized separated
husk with demineralised water; g) compacting and drying the mass; and h) sizing the compacted
mass.
In one embodiment, the process for preparation of an excipient from Trigonella foenum-graceum
seeds as per the present invention comprises: a) selecting Trigonella foenum-graecum seeds of
predetermined dimensions and swelling factor; b) roasting the seeds to facilitate separation of embryo
and husk; c) subjecting the roasted seeds to differential milling to obtain a mixture of embryo and
husk in which the embryo breaks in the form of particles; d) passing a mixture through a sieve to
substantially separate the embryo and the husk to obtain separated husk fraction containing not more
than 20% of embryo; and e) sizing of the separated husk; f) tempering/hydrating the sized separated
husk with demineralised water; g) compacting and drying the mass; h) sizing the compacted mass; i)
preparing a dispersion of sized compacted mass in acidified water and sieving it to obtain translucent
dispersion; j ) precipitating fibers from translucent dispersion with polar alcohol; k) washing
precipitate with solvents; 1) filtering and drying; and m) powdering to desired particle size.
In one embodiment, the process for preparation of an excipient from Trigonella foenum-graceum
seeds as per the present invention comprises: a) analyzing the Trigonellafoenum-graecum seed husk
or sized Trigonellafoenum-graecum seed husk for its endosperm content or water holding capacity or
swelling index or viscosity; and b) selecting husk with an endosperm content of not less than 15% or
a water holding capacity of not less than 6 g of water per g of husk or a swelling index of not less than
5 ml per g of husk or a viscosity of not less than 500 cps of 1% w/v solution.
In another embodiment, the process for preparation of an excipient from Trigonellafoenum-graceum
seeds as per the present invention comprises: a) analyzing the Trigonellafoenum-graecum seed husk
or sized Trigonellafoenum-graecum seed husk for its endosperm content or water holding capacity or
swelling index or viscosity; b) selecting husk with an endosperm content of not less than % or a
water holding capacity of not less than 6 g of water per g of husk or a swelling index of not less than
5 ml per g of husk or a viscosity of not less than 500 cps of 1% w/v solution; c) preparing a dispersion
of selected husk or selected sized husk in acidified water and sieving it to obtain translucent
dispersion; d) precipitating fibers from translucent dispersion with polar alcohol; e) washing
precipitate with solvents; f filtering and drying; and g) powdering to desired particle size.
n a still another embodiment, the process for preparation of an excipient from Trigonellafoenumgraceum
seeds as per the present invention comprises: a) analyzing the Trigonellafoenum-graecum
seed husk or sized Trigonellafoenum-graecum seed husk for its endosperm content or water holding
capacity or swelling index or viscosity; b) selecting husk with an endosperm content of not less than
% or a water holding capacity of not less than 6 g of water per g of husk or a swelling index of not
less than 5 ml per g of husk or a viscosity of not less than 500 cps of 1% w/v solution; c)
tempering/hydrating the selected husk or selected sized husk with demineralised water; d) compacting
and drying the mass; and e) sizing the compacted mass.
In a further another embodiment, the process for preparation of an excipient from Trigonellafoenumgraceum
seeds as per the present invention comprises: a) analyzing the Trigonellafoenum-graecum
seed husk or sized Trigonellafoenum-graecum seed husk for its endosperm content or water holding
capacity or swelling index or viscosity; b) selecting husk with an endosperm content of not less than
1 % or a water holding capacity of not less than 6 g of water per g of husk or a swelling index of not
less than 5 ml per g of husk or a viscosity of not less than 500 cps of 1% w/v solution; c)
tern pering/hyd rating the selected husk or selected sized husk with demineralised water; d) compacting
and drying the mass; e) sizing the compacted mass; f preparing a 2% w/v dispersion of sized
compacted mass in acidified water and sieving it to obtain translucent dispersion; g) precipitating
fibers from translucent dispersion with polar alcohol; h) washing precipitate with solvents; i) filtering
and drying; and j ) powdering to desired particle size.
Another embodiment relates to a process for preparation of excipient of the present invention
comprising a) selecting husk with an endosperm content of not less than 15% or a water holding
capacity of not less than 6 g of water per g of husk or a swelling index of not less than 5 ml per g of
husk or a viscosity of not less than 500 cps of 1% w/v solution; b) tempering/hydrating the selected
husk with demineralised water; c) compacting and drying the mass; d) sizing the compacted mass to
obtain excipient of the present invention comprising not less than 50% dietary fibers with ratio of
insoluble dietary fibers to soluble dietary fibers of about 0.2 to 1 and protein content of not more than
10 weight%.
Another embodiment relates to a process for preparation of excipient of the present invention
comprising a) selecting husk with an endosperm content of not less than or a water holding
capacity of not less than 6 g of water per g of husk or a swelling index of not less than 5 ml per g of
husk or a viscosity of not less than 500 cps of 1% w/v solution; b) preparing a 2% w/v dispersion of
selected husk in acidified water and sieving it to obtain translucent dispersion; c) precipitating fibers
from translucent dispersion with polar alcohol; d) washing precipitate with solvents; e) filtering and
drying; f) powdering to desired particle size to obtain excipient of the present invention comprising
not less than 50% dietary fibers with ratio of insoluble dietary fibers to soluble dietary fibers of about
0.2 to and protein content of not more than 0 weight%.
Still another embodiment relates to a process for preparation of excipient of the present invention
wherein the husk can be employed in the form of separated endosperm and testa combined in various
proportions ranging from but not limited to :99 to 99: 1 to prepare the desired excipient.
In one embodiment the excipient of the present invention has the following characteristics.
Parameter Results
Dietary fibers 50-85%
Insoluble dietary fibers (IDF) 20-35%
Soluble dietary fibers (SDF) 25-85%
IDF/SDF > 0.2 and < 1
Protein content <10%
Viscosity at 2%w/v at 25°C using >10,000 cps
Brookfield viscometer
Water holding capacity >20 g of water/g of excipient
Swelling Inde > 15 m /g of excipient
In another embodiment the excipient of the present invention has the following characteristics.
In still another embodiment the excipient of the present invention is characterized as follows.
Parameter Results
Dietary fibers 50-98%
Insoluble dietary fibers (IDF) 15-35%
Soluble dietary fibers (SDF) 25-75%
IDF/SDF > 0.2 and < 1
Protein content <10%
Viscosity at 2%w/v at 25°C > 10,000 cps
using Brookfield viscometer
Water holding capacity >8g of water/g of excipient
Swelling Index >6 ml/g of excipient
In yet another embodiment the excipient of the present invention is characterized as shown beneath.
The excipient of the present invention has unique properties in terms of dietary fiber content, ratio of
insoluble to soluble dietary fiber, low protein content (despite of using minimum solvent and no
lipophilic solvents like hexane and chloroform used) and desirable viscosity, water holding capacity
or swelling index. Due to these features the excipient of this invention can be employed as an
excipient in various pharmaceutical or cosmetic compositions and food, nutritional or dietary
preparations. In one aspect the present invention relates to the use of the disclosed excipient in
various pharmaceutical or cosmetic compositions and food, nutritional or dietary preparations. This
excipient has a unique chemistry, having not only galactomannan but also celluloses, and
hemiceiluiose, which contribute to the unique properties of the excipient. The excipient provided by
the present invention is effective as a release-retarding polymer, disintegrant, binder, suspending
agent, gelling agent, film forming agent, diluent and the like in pharmaceutical products and is also
useful as a stabilizer, emulsifier, dispersant or rheology modifier in personal care, food, household
care a d industrial products. The excipient acts as a good release-retarding polymer for drugs with
varying solubilities, particularly for highly soluble drugs, which are difficult to formulate in
controlled release formulation. It also acts as a good suspending agent. It can be used in all liquid,
semisolid and solid dosage forms. It can be formulated for oral, nasal, ocular, urethral, buccal,
transmucosal, vaginal, topical or rectal delivery.
The word "excipient" as used herein implies pharmaceutically or physiologically inactive additive
used in the manufacture of a pharmaceutical, cosmetic or nutritional composition or food or dietary
preparations. In one embodiment the excipient of the present invention can be added to healthcare,
personal care, food, household care or industrial products in an amount ranging from about 0.01% to
about 95% by weight of the composition, depending on the purpose of use.
A pharmaceutical excipient allows the manufacture of a pharmaceutical formulation that provides for
the necessary bioavailability of the medicament to the patient upon the administration of the
composition. The bioavailability of a given dosage form is dependent on process variables and the
interrelationship between the various excipients and the active ingredient. In one embodiment, the
excipient of the present invention when used in solid dosage forms, can serve as, inter alia, a dry or
wet binder that is used to hold together the structure of the dosage forms. In yet another embodiment,
the excipient of the present invention can be used as disintegrant. The disintegration properties are
based upon the ability of the excipient of the present invention to swell in the presence of a fluid such
as water or gastric juice. This swelling disrupts the physical continuity of the structure of the dosage
form, leading to its physical disintegration. In another embodiment, the excipient of the invention can
be used as thickening agents in syrups, suspensions, emulsions or in syrups or suspensions for
reconstitution. One of the important aspects of these dosage forms is the viscosity, which is required
to prevent sedimentation rate of the solids in suspension and to achieve desired stability in case of
emulsion and to arrive at a consistency suitable for administration in case of solutions. Thickening
agent such as dietary fiber rich excipient imparts viscosity and is therefore an important additive in
these formulations. The actual concentration of the excpient of the present invention can be selected
based on the desired consistency. In still another embodiment, the excipient of the invention can be
used as stabilizer for liquid dosage forms. It can be used as a suspending agent or as an emulsifying
agent. It can also be employed as a thickening agent, base or gelling agent for these semisolid
formulations. The concentration can be selected based on the desired consistency, appearance and the
desired physical and chemical properties of the final product. In another embodiment, the excipient of
the invention can be used as a coating agent for protecting the medicinal agent against destructive
exposure to air and/or humidity, mask the taste of the drug, provide special characteristics of drug
release and to provide aesthetic or distinction to the product. Commonly employed plasticizers such
as polyethylene glycol, opacifiers or colorants can be used along with the excipient of the present
invention for coating. In a further embodiment, the excipient of the invention can be used as release
retarding polymer. The concentration of the excipient is based on the desired release profile, and the
nature and dose of the active pharmaceutical ingredient. The excipient of the present invention can be
used alone or in combination with the said polymers. The excipient of the present invention can be
effectively used for drugs with varying solubilities and for controlled delivery of both lipophilic and
hydrophilic drugs. Also, the excipient of the invention can be conveniently employed for large,
medium and low dose drugs, alone or in combination. It can be incorporated in the various dosage
forms that can be used for controlling the drug release such as capsules, tablets, micro granules,
pellets, coated systems, etc. Further the excipient of the present invention can be employed for its
polymeric and film forming property in the manufacturing of soft gelatin capsules. The excipient of
the present invention can also act as an effective excipient in gastroretentive dosage forms. In yet
another embodiment, the excipient of the invention can be used as structural component in films,
devices or patches for transdermal applications. In a further embodiment the excipient can be
incorporated in the following dosage forms: a capsule, a tablet, an ovule, a suppository, an insert, a
wafer, a chewable tablet, a buccal tablet, a sublingual tablet, a quick-dissolve tablet, an effervescent
tablet, a granule, a pellet, a bead, a pill, a sachet, a sprinkle, a film, an ointment, a cream, a gel, a dry
syrup, a reconstitutable solid, a suspension, an emulsion, a lozenge, a troche, an implant, a powder, a
triturate, a platelet, or a strip. These pharmaceutical compositions can be formulated for immediate
release, pulsatile release, controlled release, extended release, modified release, delayed release,
targeted release, or targeted delayed release. Also the compositions can be formulated for oral, nasal,
ocular, urethral, buccal, transmucosal, vaginal, topical or rectal delivery. For development of these
dosage forms this excipient can be combined with other excipients such as water soluble polymer,
water insoluble polymers, hydrophobic materials, hydrophilic materials, waxes, disintegrants,
superdisintegrants, diluents, binders, etc.
In a further embodiment the excipient of the present invention can be used in food, nutritional, dietary
or personal care compositions as a stabilizer, emulsifier, dispersant or rheology modifier. It can also
be used in household and industrial products as well. The excipient of the present invention can also
be employed in cosmetic or personal care compositions to stabilize lotions and protective creams. It
can also be used to increase the viscosity, assist in imparting spreading, add a smooth feel to the skin,
and form a protective coating. The excipient of the present invention can also be used in personal care
(such as, for example, hair and skin) products, to aid wetting of the skin, scalp or hair, facilitate dirt
removal and dissolution, and ease rinsing after application. The excipient of the present invention can
thus be used in personal care products as rheology modifiers, stabilizers^ emulsifiers, binders,
dispersants or film formers.
I the food industry, especially during the manufacture of ice creams, ice cream shakes and frozen
desserts the excipient of the present invention can be used as stabilizer to maintain homogeneity,
control ice crystal growth during the freezing or aeration process, and to provide slower and more
uniform meltdown. The excipient of the present invention due to desirable water holding capacity is
capable of binding quantities of water considerably larger than their weight and retarding the growth
of ice crystals when the frozen food is subject to changes in temperature. Further, the excipient
provides smooth texture and stability to dairy products and maintains their optimum quality for
extended time periods. It can also help reduce syneresis in dairy products and prevent moisture
migration. The excipient can be employed in baked foods to provide improved texture, mouth feel,
softness, moisture-retention, shelf-life and fatty attributes to them. The excipient of the present
invention can also be used to encapsulate flavors that are used in foods. In confectionaries the
excipient of the present invention can be used as a stabilizer by retarding sugar crystallization or as
emulsifiers and dispersants by emulsifying and distributing fat particles in the confectionary product.
The excipient can also be utilized in the beverage industry to stabilize flavors and essential oils. The
synergistic presence of fenugreek soluble dietary fiber and insoluble dietary fiber provides enhanced
emulsification and stabilization properties and also serves as cloud-producing agent and foamstabilizing
agent in the beverage industry.
The excipient of the present invention can thus be used in food, fodder, pharmaceutical, personal care,
household care and industrial products. It can be used in these products for various functions, without
being limited only to the above mentioned list of applications.
While the present invention has been described in terms of its specific embodiments, certain
modifications and equivalents will be apparent to those skilled in the art and are intended to be
included within the scope of the present invention. The following examples merely illustrate the
present invention and are not to be construed to limit, in any way, the scope of the invention.
Examples:
1) Process for preparation of excipient of the present invention
5 kg Fenugreek seeds were purchased from a local source (Mumbai, India). Seeds were roasted using
flaking drum wherein the seeds were roasted in a rotating drum at temperature of 80°C. Roasted seeds
were introduced into the roller mill in a continuous process. The milled material was then collected
and passed through a 16# sieve to substantially separate the embryo and the husk to obtain a husk
fraction containing 3% of embryo. The amount of yellow embryo fraction in the separated husk was
determined by physical separation of embryo remnants from the husk fraction. The separated husk (~
3.5 kg) was hydrated by using about 50% demineralised water for about 90 minutes. Roll compaction
of this hydrated husk was further earned out. The roll compacted mass was dried using fluidized bed
dryer to loss on drying of less than about 2% and the compacted mass was then sized by milling to
obtain 1 kg of excipient (I) of the present invention with not less than 65% having a particle size
<250.
2) Process for preparation of excipient of the present invention
Fenugreek husk samples obtained from local sources were analyzed for their viscosity. Husk with a
viscosity of not less than 500 cps of l%w/v solution was selected for the preparation of excipient. The
selected husk (~ 5 kg) was hydrated by using about 50% demineralised water for about 90 minutes
with mixing. Roll compaction of this hydrated husk was further carried out. The roll compacted mass
was dried using fluidized bed dryer to loss on drying of less than about 2% and the compacted mass
was then sized by milling to obtain 1.4 kg of excipient (II) of present invention with not less than
65% having a particle size <250.
3) Process for preparation of excipient of the present invention
5 kg Fenugreek seeds were purchased from a local source (Mumbai, India). Seeds were roasted using
flaking drum wherein the seeds were roasted in a rotating drum at temperature of 80°C. Roasted seeds
were introduced into the roller mill in a continuous process. The milled material was then collected
and passed through a 6# sieve to substantially separate the embryo and the husk to obtain a husk
fraction. A dispersion of 250 g of the separated husk was prepared in acetic acid under stirring for
hr. The dispersion thus obtained was filtered through a 60# sieve to separate the dispersion from
insoluble mass. The water insoluble fraction was again subjected to extraction for better recovery. All
fractions were combined to give a volume of about 35 L. The dispersion thus obtained was treated
with approximately half the quantity of methanol (-18 L), which resulted in the precipitation of
dietary fibers. The white hairy mass thus obtained was filtered. Since the filtered white mass contains
water bound to it, which may affect the properties of the final product and cause difficulty in drying
the mass to obtain a powder, the moisture was removed by treating the fibers with acetone with
neutralization step in between. Final washing of the product was given with acetone. The washed
material thus obtained was dried at 60°C for 9 hrs and powdered to obtain a 60# fraction of excipient
(III) of the present invention.
4) Characterization of excipient of the present invention
Characterization of excipient (3 samples) of the present invention prepared in examples 1, 2 and 3
above has been shown beneath in Table 1.
Table 1
No. Parameter Excipient (I) of Excipient Excipient Test Method
the present (II) of the (III) of the
invention present present
invention invention
1. Dietary fibers 90.09 90.21 94.20 AOAC 8th
(%w/w) edition 2007,
985.29
Insoluble dietary 31.80 28.48 23.05 AOAC 8 h
fibers edition 2007,
(IDF) (%w/w) 993.19
Soluble dietary 62.40 6 1.73 67.04 AOAC 8,
fibers edition 2007,
(SDF) (%w/w) 991.42
IDF/SDF 0.50 0.46 0.34
2 . Protein content 5.5 3.9 4.9 AOAC 8 h
(%w/w) edition 2007,
984.13
3 . Viscosity (cps) 1,00,000 1,10,000 1,60,000 At 2%w/v at
25°C using
Brookfleld
viscometer
4 . Water holding 12 14 30.83 Centrifugation
capacity and filtration
(g of water/g of method
excipient)
5. Swelling Index 8.33 9.5 22 Ph.Eur 6.0
(ml/g of
excipient)
5) Comparative evaluation of viscosity, water holding capacity and swelling index of excipient
of the present invention with commercial products
(a) Comparative data of viscosities
The viscosity of a l%w/v solution of excipient (111 of example 3) of the present invention,
hydroxypropyl methylcellulose (Methocei K100M® and Methocei K4M® (obtained from Dow
chemicals)), guar gum (Supercol Kl), psyllium husk (Isaphagula) and Nutriose® (soluble fiber) was
compared. 1% w/v solution of these polymers was prepared in distilled water and kept overnight for
deaeration. Their viscosities were then determined at 25°C using Brookfield viscometer LV model
and are indicated below in Table 2 .
Table 2
No. Polymers Viscosity in cps
1 Methocei K100M 2700
2 Methocei K4M 160
3 Guar gum 710
4 Psyllium liusk 862.5
5 Nutriose® (soluble fiber) 3
6 Excipient of the present 10,000
invention (III of example 3)
This data suggests that the excipient of the present invention exhibited maximum viscosity compared
to all other gums or polymers. This indicates that the excipient of the present invention can act as an
effective controlled release excipient or a rheology modifier.
(b) Comparative data of swelling index
The swelling index is the volume in millilitres occupied by 1 gram of test material after it has swollen
in an aqueous liquid for 4 h. The swelling index of the excipient of the present invention was
compared against that of guar gum (Supercol ), psyllium husk (Isaphagula) and Nutriose® (soluble
fiber) using the method laid down in European Pharmacopoeia 6.0. The method involved placing .0g
of the test material in a 25ml ground-glass stoppered cylinder, which are shaken vigorously every 0
minutes for 1 hour and then allowed to stand for 3 hours. The volume occupied by the test material is
measured, including any adhering mucilage. The results as depicted in the table 3 beneath clearly
indicate that the swelling index of excipient is better than the other gums or fibers and comparable to
psyllium husk.
Table 3
This data indicates that the excipient of the present invention has high swelling index and can act as
an effective excipient in gastroretentive dosage forms.
(c) Comparative data of water holding capacities
The water holding capacity of material is a measure of the ability of the material to immobilize water
within its matrix. The centrifugation and filtration method was used to compare the water holding
capacity of the excipient of the present invention against that of guar gum (Supercol Kl), psyllium
husk (Isaphagula) and Nutriose® (soluble fiber). For the centrifugation method tared centrifuge tubes
each containing the specified amounts of material soaked for 24 h in distilled water were centrifuged
at 10000 rpm for 20 min and the supernatant fraction was decanted. The fresh weight of material was
determined and the water holding capacity was calculated as g water/g material. The results obtained
as depicted beneath in table 4 clearly indicate that excipient of the present invention has a better water
holding capacity than the other comparators.
Table 4
This data indicates that the excipient of the present invention can act as an effective ingredient in food
and dietary preparations.
6) Use of excipient of the present invention as a controlled release agent
Excipient of the present invention can be used as a controlled release agent for a highly water soluble
drug - propranolol hydrochloride as described in table 5 beneath.
Table 5
Ingredients Lot A (mg/unit) Lot B (mg/unit)
Propranolol hydrochloride 160 160
Hydroxypropyl methyl cellulose, USP
160
(Methocel® K 100M)
Excipient III of example 3 - 160
Magnesium stearate, USP 1.6 1.6
Colloidal silicon dioxide, USP 3.4 3.4
Total 325 325
Propranolol hydrochloride in Lot A was blended with hydroxypropyl methyl cellulose and colloidal
silicon dioxide and in Lot B was blended with the excipient of the present invention and colloidal
silicon dioxide. The two lots were then compressed into tablets after lubrication with magnesium
stearate. Dissolution was carried out in USP apparatus 11 (paddle) at 50 rpm using 900 ml dissolution
media with 0.1N hydrochloric acid for 2 hours followed by dissolution testing in p 6.8 phosphate
buffer.
The dissolution profile is as indicated in the table 6 beneath.
Table 6
Time intervals Average %release
(hrs) Lot A Lot B
1 21.1 20.5
2 30.7 3 1.8
4 35.1 35.9
6 45.4 46.1
8 55 56.3
12 64.5 65
14 69.3 70.5
From the above data it can be concluded that the excipient of the present invention can be used as a
controlled release agent for highly water-soluble drug such as propranolol hydrochloride. The release
retarding properties of the excipient of the present invention are seen to be comparable to that of
hydroxypropyl methyl cellulose.
7) Use of excipient of the present invention as a binder
Binding properties of the excipient of the present invention were compared against those of
commercially used binders such as polyvinylpyrrolidone and copovidone. Tramadol hydrochloride
was used as a model drug for this study. The drug was granulated using 1% binder solution with
formulation A employing the excipient (111 of example 3) of the present invention as a binder,
formulation B employing polyvinylpyrrolidone as a binder and formulation C employing copovidone
as a binder, the formed granules were then blended with the remaining ingredients and then lubricated
and compressed.
Table 7
The above data shows that the physical parameters such as hardness, friability and disintegration time
of the three formulations are comparable and therefore it can b e concluded that the excipient of the
present invention has good binding properties.
8) Evaluation of the saponin content of the excipient of the present invention
The saponin content of the excipient of the present invention (111 of example 3) was analyzed using
HPLC method and the saponin content was found to be 0.92 weight %.
This data indicates that the excipient of the present invention has low saponin content as and therefore
can be used as an excipient in pharmaceutical and cosmetic compositions.
CLAIMS
1) An excipient obtained from Trigonellafoenum-graceum seeds comprising:
dietary fibers in an amount of not less than about 50% by weight of the excipient, wherein said
dietary fibers have a ratio of insoluble dietary fibers to soluble dietary fibers of about 0.2 to about
1; and
a protein content of not more than about 0% by weight of the excipient.
2) The excipient according to claim 1, wherein said dietary fibers are present in an amount of about
50% by weight to about 98% by weight of the excipient.
3) The excipient according to claim 1, wherein the ratio of insoluble dietary fibers to soluble dietary
fibers is about 0.2 to about 0.8.
4) The excipient according to claim 1, wherein the ratio of insoluble dietary fibers to soluble dietary
fibers is about 0.2 to about 0.7.
5) The excipient according to claim 1, wherein the ratio of insoluble dietary fibers to soluble dietary
fibers is about 0.3 to about 0.8.
6) The excipient according to claim , wherein said excipient has a viscosity greater than 10,000 cps
at 2%w/v concentration at 25°C.
7) The excipient according to claim 1, wherein said excipient has a swelling index of greater than
about 6ml/gram of excipient.
8) The excipient according to claim 1, wherein said excipient has a water holding capacity of greater
than about 8 grams of water per gram of excipient.
9) A process for preparation of an excipient from Trigonellafoenum-graceum seeds as claimed in
claim 1 comprising:
a) selecting Trigonellafoenum-graecum seeds of predetermined dimensions and swelling factor;
b) roasting the seeds to facilitate separation of embryo and husk;
c) subjecting the roasted seeds to differential milling to obtain a mixture of embryo and husk in
which the embryo breaks in the form of particles;
d) passing a mixture through a sieve to substantially separate the embryo and the husk to obtain
separated husk fraction contain ing not more than 20% of embryo; and
e) sizing of the separated husk.
10) The process according to claim 9, further comprises:
f) preparing a dispersion of sized separated husk in acidified water and sieving it to obtain
translucent dispersion;
g) precipitating fibers from translucent dispersion with polar alcohol;
h) washing precipitate with solvents;
i) filtering and drying; and
j ) powdering to desired particle size.
11) The process according to claim 9, further comprises:
f ) tempering/hydrating the sized separated husk with demineralised water;
g) compacting and drying the mass; and
h) sizing the compacted mass.
12) The process according to claim 1, further comprises:
i) preparing a dispersion of sized compacted mass in acidified water and sieving it to obtain
translucent dispersion;
j ) precipitating fibers from translucent dispersion with polar alcohol;
k) washing precipitate with solvents;
1) filtering and drying; and
) powdering to desired particle size.
13) A process for preparation of an excipient from Trigonellafoenum-graceum seeds as claimed in
claim 1 comprising:
a) analyzing the Trigonellafoenum-graecum seed husk or sized Trigonellafoenum-graecum seed
husk for its endosperm content or water holding capacity or swelling index or viscosity; and
b) selecting husk with an endosperm content of not less than % or a water holding capacity of
not less than 6 g of water per g of husk or a swelling index of not less than 5 ml per g of husk or a
viscosity of not less than 500 cps of 1% w/v solution.
14) The process according to claim 3, further comprises:
c) preparing a dispersion of selected husk or selected sized husk in acidified water and sieving it
to obtain translucent dispersion;
d) precipitating fibers from translucent dispersion with polar alcohol;
e) washing precipitate with solvents;
f) filtering and drying; and
g) powdering to desired particle size.
) The process according to claim 3, further comprises:
c) tempering/hydrating the selected husk or selected sized husk with demineralised water;
d) compacting and drying the mass; and
e) sizing the compacted mass.
16) The process according to claim 5, further comprises:
f preparing a dispersion of sized compacted mass in acidified water and sieving it to obtain
translucent dispersion;
g) precipitating fibers from translucent dispersion with polar alcohol;
h) washing precipitate with solvents;
i) filtering and drying; and
j ) powdering to desired particle size.
17) Use of an excipient from Trigonellafoenum-graceum seeds as claimed in claim 1 for preparation
of pharmaceutical or cosmetic compositions and food, nutritional or dietary preparations.