DESC:FORM 2

THE PATENTS ACT 1970
(SECTION 39 OF 1970)

&
THE PATENT RULES, 2003

COMPLETE SPECIFICATION
(SECTION 10)

FENUGREEK POWDER AND ITS COMPOSITIONS

We, AZISTA INDUSTRIES PVT LTD,
a company incorporated under the company’s Act, 1956 having address at
Sy.No. 80-84, 4th Floor, C Wing, Melange Towers, Patrika Nagar, Madhapur, Hyderabad, Telangana- 500081, India

The following specification particularly describes the invention and the manner in which it is to be performed:

FIELD OF INVENTION
The present invention relates to Fenugreek powder with high trigonelline, saponin, 4-hydroxyisolueucine, galactomannans and secondary metabolic phytochemical contents. The present invention specifically relates to a novel process for preparation of Fenugreek powder with high trigonelline, saponin, 4-hydroxyisolueucine, galactomannans & other phytochemical contents.

The present invention more specifically relates to compositions containing fenugreek powder and process for the preparation thereof which reduces the diabetes mellitus, bone associated pain, brain associated disorder and erectile dysfunction.

BACKGROUND OF INVENTION
Fenugreek is an annual leguminous plant. Fenugreek seeds are known to have been used for long time for traditional spices such as curry powder. In the ancient history of Ayurveda, Fenugreek seeds considered as a potent medicine for the treatment of multiple disorders.

Fenugreek (Trigonella foenum-graecum) has attracted considerable interest as a natural source of soluble dietary fiber and diosgenin (sapogenins). The fenugreek seed contains a central hard, yellow embryo surrounded by a corneous and comparatively large layer of white, semi-transparent endosperm. This endosperm contains galactomannan gum. The endosperm is surrounded by a tenacious, dark brown husk. The color of the gum fraction depends upon the amount of outer husk (brown color) and cotyledon (yellow color) present.

Fenugreek is one of the popular seeds to grow as sprouts for a nutritious addition to salads or freshly juiced vegetable blends. Like other sprout varieties including, sunflower, radish, alfalfa and broccoli sprouts, when these types of seeds are sprouted they provide a highly concentrated source of energy, packed with pre-digested vitamins, minerals, protein-rich amino acids, sugars and fatty acids.
Fenugreek sprouts contain trigonelline which is a plant hormone that has diverse regulatory functions with respect to plant cell cycle regulation, nodulation, and oxidative stress, and in helping survival and growth of the plant. The chemical formula for trigonelline is C7H7NO2. It is a methylation product of niacin (vitamin B3), and thus is also known as “methylated niacin.” At higher temperatures, trigonelline breaks down to niacin. In addition to trigonelline, fenugreek sprouts also contain other alkaloids such as gentianine and carpaine.

Trigonelline reduces blood glucose in humans. Trigonelline protects-cells of the pancreas and increases insulin sensitivity index as well as insulin content.

US 6,495,175 B2 discloses a method for obtaining substantially pure fixed oil(s), oleoresin and dietary fiber from Fenugreek seeds. The method employs two different solvent extraction stages, wherein the first extraction isolates fixed oils and the second extraction isolates oleoresin.

CN 102697781 B discloses use of trigonelline in the manufacture of diabetes and its complications medicaments. This patent also discloses trigonelline compositions in the form of oral tablet or capsule and the like.

Wani et al., Journal of the Saudi Society of Agricultural Sciences, 2018, 17, 97-106 discloses medicinal qualities of Fenugreek such as antidiabetic, anticarcinogenic, hypocholesterolemic, antioxidant, and immunological activities. Seeds of fenugreek spice have medicinal properties such as hypocholesterolemic, lactation aid, antibacterial, gastric stimulant, for anorexia, antidiabetic agent, galactogogue, hepatoprotective effect and anticancer. Chemical constituents of fenugreek includes
a) Alkaloids like trimethylamine, neurin, trigonelline, choline, gentianine, carpaine and betain. b) Aminoacids like isoleucine, 4-hydroxyisoleucine, histidine, leucine, lysine, L-tryptophan, arginine. c) Saponins like Graecunins, fenugrin B, fenugreekine,
trigofoenosides A–G. d) Steroidal sapinogens like Yamogenin, diosgenin, smilagenin,
sarsasapogenin, tigogenin, neotigogenin, gitogenin, neogitogenin, yuccagenin, saponaretin. e) Flavonoids like quercetin, rutin, vitexin, isovitexin. f) Fibers like Gum, neutral detergent fiber. g) Lipids like triacylglycerols, diacylglycerols, monoacylglycerols, phosphatidylcholine phosphatidylethanolamine, phosphatidylinositol, free fatty acids. h) Others like coumarin, lipids, vitamins, minerals, 28% mucilage, 22% proteins, 5% of a stronger swelling, bitter fixed oil.

All prior art documents discloses the extraction of different components from the Fenugreek seeds and use of trigonelline in the treatment of diabetes mellitus, use of Fenugreek in the treatment of anticarcinogenic, hypocholesterolemic, antioxidant, and immunological activities. However, the inventors of the present invention have developed a new method for the preparation of Fenugreek powder with high trigonelline, saponin, 4-hydroxyisoleucine, galactomannans contents from the Fenugreek sprouts. The inventors of present invention have also prepared the final dosage forms comprising of Fenugreek powder with high trigonelline, saponin, 4-hydroxyisoleucine, galactomannans contents for treatment of diabetes mellitus, bone associated pain, brain associated disorder and erectile dysfunction.

OBJECTIVE OF INVENTION
The main objective of the present invention is to develop Fenugreek powder using novel technology with high trigonelline, saponin, 4-hydroxyisoleucine, galactomannans & other phytochemical contents.

Another objective of the present invention is to provide a novel process for the preparation of Fenugreek powder with high trigonelline, saponin, 4-hydroxyisoleucine, galactomannans & other associated phytochemical contents.

Another objective of the present invention is to provide compositions of Fenugreek powder and process for the preparation of different formulations thereof for the treatment of diabetes mellitus, brain associated disorders, joint pain, gastrointestinal disorder & erectile dysfunction.

SUMMARY OF INVENTION
Accordingly, the present invention relates to a fenugreek powder with high trigonelline, saponin, 4-hydroxyisoleucine, galactomannans and other phytochemical contents.

Another embodiment of the present invention relates to a novel process for the preparation of Fenugreek powder with high trigonelline, saponin, 4-hydroxyisoleucine, galactomannans & other phytochemical contents.

Another embodiment of the present invention relates to a novel process for preparation of Fenugreek powder using advanced sprouting of fenugreek which contains more trigonelline, saponin, 4-hydroxyisoleucine, galactomannans contents than Fenugreek powder obtained from other methods.

Another embodiment of the present invention relates to a novel process for preparation of Fenugreek powder, wherein the process comprising raw seed optimization, seed treatment, soaking of seed in water, incubation in growth chamber, termination of seed growth and powder preparation.

Another embodiment of the present invention relates to a novel process for preparation of Fenugreek powder comprising;
a) collecting fenugreek seeds from different regions,
b) treating seeds with surfactants to decrease the microbial load from the fenugreek seeds and accelerate the germination process,
c) soaking treated seeds in Reverse Osmosis water & ground water at -5 PSI to 50 PSI up to the 4Hrs to 24 Hrs with various temperature range from 20 – 50 degree,
d) incubating soaked seeds upto 12 days,
e) sampling germinated seeds from day 1 to day 12 and evaluating for trigonelline, saponin, 4-hydroxyisoleucine, galactomannans and other phytochemical contents,
f) terminating the seed growth after or in between 12 days, and
g) preparing the dry powder from raw sprout material.

Another embodiment of the present invention relates to compositions of fenugreek powder comprising one or more excipients.

Another embodiment of the present invention relates to a fenugreek tablet comprising one or more pharmaceutically acceptable excipients, wherein the tablet is optionally coated with polymers.

Yet another embodiment of the present invention relates to a fenugreek tablet comprising one or more pharmaceutically acceptable excipients selected from binders, diluents, fillers, disintegrants, lubricants and flavouring agents.

Yet another embodiment of the present invention relates to a fenugreek tablet composition comprising one or more excipients selected from polyethylene glycol, dibasic calcium phosphate, sodium starch glycollate, colloidal silicon dioxide and magnesium stearate.

Yet another embodiment of the present invention relates to a process for the preparation of fenugreek tablet comprising;
a) sifting the fenugreek powder through sieve,
b) preparing the binder solution by dissolving binder in purified water,
c) granulating the fenugreek powder with above binder solution,
d) milling and drying the granules,
e) adding extra-granular excipients to the above granules,
f) compressing the granules into tablets, and
g) optionally, coating the tablets with film coating or sugar coating.

Yet another embodiment of the present invention relates to fenugreek capsule comprising one or more pharmaceutically acceptable excipients selected from binders, diluents, fillers, disintegrants, lubricants and flavouring agents.

Yet another embodiment of the present invention relates to fenugreek capsule composition comprising fenugreek powder and one or more excipients selected from polyethylene glycol, dibasic calcium phosphate, sodium starch glycollate, colloidal silicon dioxide and magnesium stearate.

Yet another embodiment of the present invention relates to a process for the preparation of fenugreek capsules comprising;
a) sifting fenugreek powder through sieve,
b) dissolving the binder in purified water to make binder solution,
c) granulating the fenugreek powder using above binder solution,
d) milling and drying the granules,
e) adding extra-granular excipients to the above granules and mixing,
f) filling the granules into capsules.

Yet another embodiment of the present invention relates to fenugreek syrup containing fenugreek powder and one or more pharmaceutically acceptable excipients.

Yet another embodiment of the present invention relates to fenugreek syrup composition comprising fenugreek powder and one or more excipients selected from carriers, solubilizers, stabilizers, sweeteners, preservatives and flavouring agents.

Yet another embodiment of the present invention relates to fenugreek syrup composition comprising fenugreek powder and one or more excipients selected from propylene glycols, polyvinylpyrrolidone, sucrose, saccharin sodium and sodium benzoate.

Yet another embodiment of the present invention relates to a process for the preparation of fenugreek syrup comprising;
a) adding the fenugreek powder to the carriers to obtain a solution,
b) adding sweeteners, solubilizers, preservatives and flavouring agents to the water to obtain a solution,
c) mixing these solutions to obtain the syrup.

Still yet another embodiment of the present invention provides equipment for the sprouting of fenugreek seeds.

DETAILED DESCRIPTION OF THE INVENTION
The term "comprising", which is synonymous with "including", "containing", or "characterized by" here is defined as being inclusive or open-ended, and does not exclude additional, unrecited elements or method steps, unless the context clearly requires otherwise.

The Fenugreek composition of the present invention can be used for the treatment of different conditions of humans includes pro-inflammatory diseases including cancer, cardiovascular disease, arthritis, uveitis, ulcerative proctitis, Crohn’s disease, ulcerative colitis, irritable bowel disease, tropical pancreatitis, peptic ulcer, gastric ulcer, idiopathic orbital inflammatory pseudotumor, oral lichen planus, gastric inflammation, vitiligo, psoriasis, acute coronary syndrome, atherosclerosis, diabetes, diabetic nephropathy, diabetic microangiopathy, lupus nephritis, renal conditions, acquired immunodeficiency syndrome, ß-thalassemia, biliary dyskinesia, dejerine-sottas disease, cholecystitis, neurological disorders, dyslipidaemia, and chronic bacterial prostatitis.

In other embodiment, the fenugreek powder of the present invention is prepared by method comprising:
1. Fenugreek seeds were collected from different regions of India i.e. North, South East & West. Fenugreek Seed variety was optimized on the basis of the quality of germination rate, and quantity of trigonelline, saponin, 4-hydroxyisoleucine, galactomannans and other phytochemical contents.
2. Seed treatment process was used to decrease the microbial load from the fenugreek seeds and accelerate the germination process. Some surfactants were optimized for the fenugreek seeds for its microbes’ free germination i.e. H2O2, HOCl, SDS, Ethanol, UV and Sonication with different time of exposure/strength.
3. Treated seed were soaked in to the RO water at -5 PSI to 50 PSI up to the 4Hrs to 24 Hrs with various temperature range from 20 – 50 degree. Light cycle during the soaking period was also evaluated i.e. Light / Dark.
4. Soaked seeds were transferred onto the mesh (8 mm/10mm/12 mm/14 mm/16 mm) made up by the plastic/SS/Nylon/Cotton and sterile pressure/pure oxygen applied from - 5PSI to 50 PSI. The temperature for the incubation was optimized between the range of 15 – 50 degree. RH was maintained from 40% to 90%.
5. Continuous Samplings of the germinated seeds were taken for their growth & phytochemical analysis from day 1 to day 12. Saponin/Trigonelline/ Antioxidant/Amylase/Vitamin/Protein/Fat/Carbohydrate and micronutrients were quantified up to the 12th days. Trigonelline content was found 9 times higher at the optimized phase of seed germination compared with raw seeds.
6. Cotyledon and Radical of the germinated seeds were examined up to the 12th day of germination for the better yield of the essential phytochemical. Non-essential components were excluded out in order to develop an ameliorative product. Raw sprout material further extracted with the organic and inorganic solvent for the purity of phytochemicals.

Other additives used in the preparations of the compositions of the present invention, the following can be used and there were no limitations: stabilizer, surfactant, plasticizer, lubricant, reducing agent, buffer agent, sweetening agent, base, adsorbent, corrigent, binder, suspending agent, antioxidant, polish, coating, wetting agent, wet modifier, filler, antifoaming agent, refrigerative agent, coloring matter, flavoring agent, perfume, sugar coating agent, isotonizing agent, softener, emulsifying agent, foaming agent, pH modifier, anti-frothing agents, diluent, excipient, dispersing agent, disintegrator, fragrance, desiccant, antiseptics, preservative, solubilizing agent, solubilizer, solvent, superplasticizer, antistatic agent, extender, moisturizing agent, and the like.

Binders used in the present invention are selected from the group consisting of cellulose polymers (such as hydroxypropylmethyl cellulose, hydroxypropyl cellulose, hydroxyethyl cellulose, ethyl cellulose, and methyl cellulose), gelatin, pregelatinized starch, acacia, alginic acid, sodium carboxymethyl cellulose gum arabic, polyvinylpyrrolidone, polyethylene glycols, polyvinyl alcohol, copolymers of N-vinyl pyrrolidine and vinyl acetate and mixtures thereof. Preferably, the binder is selected from the group consisting of cellulose polymers (such as hydroxypropylmethyl cellulose, hydroxypropylcellulose, methylcellulose and hydroxyethyl cellulose), polyvinylpyrrolidone, polyvinyl alcohol and mixtures thereof, and more preferably the binder is selected from the group consisting of hydroxypropylmethyl cellulose, hydroxypropyl cellulose, hydroxyethyl cellulose, ethyl cellulose, methyl cellulose, polyvinyl pyrrolidone, polyvinyl alcohol, and mixtures thereof.

Diluents or fillers used in the present invention are selected from the group consisting of microcrystalline cellulose, powdered cellulose, lactose (anhydrous or monohydrate), compressible sugar, fructose, dextranes, other sugars such as mannitol, sorbitol, lactitol, saccharose or a mixture thereof, siliconised microcrystalline cellulose, calcium hydrogen phosphate, dibasic calcium phosphate, calcium carbonate, calcium lactate or mixtures thereof.

Disintegrants used in the present invention are selected from the group consisting of carboxymethylcellulose, carboxymethylcellulose calcium (CMC-Ca), carboxymethylcellulose sodium (CMC-Na), crosslinked sodium carboxymethyl cellulose as e.g. Ac-Di-Sol®, Primellose®, Pharmacelt® XL, Explocel®, and Nymcel® ZSX having a molecular weight of 90 000-700 000, sodium starch glycolate e.g. Explosol®, Explotab®, Glycolys®, Primojel®, Tablo®, Vivastar® P, in particular having molecular weight is 500000-11000000, crosslinked polyvinylpolypyrrolidone (Plasone-XL®, Polyplasdone® XL and Kollidon® CL) in particular having a molecular weight in excess of 1000000, more particularly having a particle size distribution of less than 400 microns or less than 74 microns, microcrystalline cellulose, L-HPC (low-substituted hydroxypropylcellulose), sodium carboxymethyl starch, sodium glycolate of potato starch, partially hydrolysed starch, wheat starch, maize starch, rice starch or potato starch, cornstarch, pregelatinized starch, crospovidone, for example, POLYPLASDONE XL® (International Specialty Products), magnesium aluminium silicate or mixtures thereof.

Lubricants used in the present invention are selected from the group consisting of stearic acid, magnesium stearate, calcium stearate, sodium lauryl sulphate, hydrogenated vegetable oil, hydrogenated castor oil, sodium stearyl fumarate, macrogols, or mixtures thereof.

Surfactants used in the present invention are selected from the group consisting of sodium salts of fatty alcohol sulphates such as sodium lauryl sulphate; or sulphosuccinates such as sodium dioctyl sulphosuccinate; or partial fatty acid esters of polyhydric alcohols such as glycerol monostearate, glyceryl monooleate, glyceryl monobutyrate; or block copolymers of ethylene oxide and propylene oxide, also known as polyoxyethylene polyoxypropylene block copolymers or polyoxyethylene polypropyleneglycol, such as Poloxamer 124, Poloxamer 188, Poloxamer 237, Poloxamer 388, Poloxamer 407 (BASF Wyandotte Corp.); or fatty acid esters of sorbitan such as sorbitan mono laurate, sorbitan monopalmitate, sorbitan monooleate, sorbitan stearate, sorbitan monolaurate etc. such as Span or Arlacel , Emsorb®, Capmul®, or Sorbester®, Triton X-200 etc.; or a fatty acid esters of polyhydroxyethylene sorbitan such as polyoxyethylene (20) sorbitan, e.g. polyoxyethylene (20) sorbitan monooleate (Tween® 80), polyoxyethylene (20) sorbitan monostearate (Tween®60), polyoxyethylene (20) sorbitan monopalmitate (Tween®40), polyoxyethylene (20) sorbitan monolaurate (Tween® 20); or polyethylene glycol fatty acid esters, e.g. PEG-200 monolaurate, PEG-200 dilaurate, PEG-300 dilaurate, PEG-400 dilaurate, PEG-300 distearate, PEG-300 dioleate; alkylene glycol fatty acid mono esters, e.g. propylene glycol monolaurate (Lauroglycol®); or hydrogenated castor oil and polyoxyethylene castor oil derivates, e.g. polyoxyethyleneglycerol triricinoleate or polyoxyl 35 castor oil (Cremophor® EL; BASF Corp.); or polyoxyethyleneglycerol oxystearate such as polyethylenglycol 40 hydrogenated castor oil (Cremophor RH® 40) or polyethylenglycol 60 hydrogenated castor oil (Cremophor RH® 60); or sucrose fatty acid esters, such as sucrose stearate, sucrose oleate, sucrose palmitate, sucrose laurate, and sucrose acetate butyrate; or vitamin E and its derivatives such as Vitamin E-TPGS® (d-alpha-tocopheryl polyethylene glycol 1000 succinate); or phospholipids, glycerophospholipids (lecithins, kephalins, phosphatidyl serine), glyceroglycolipids (galactopyransoide), sphingophospholipids (sphingomyelin), and sphingoglycolipids (ceramides, gangliosides), DSS (docusate sodium), docusate calcium, docusate potassium, SDS (sodium dodecyl sulfate or sodium lauryl sulfate), dipalmitoyl phosphatidic acid, sodium caprylate; or bile acids and salts thereof; or ethoxylated triglycerides; or quaternary ammonium salts such as cetyl-trimethylammonium bromide, cetylpyridinium chloride; or glycerol acetates such as acetin, diacetin and triacetin; or triethanolamine, lecithin, monohydric alcohol esters such as trialkyl citrates, lactones and lower alcohol fatty acid esters, nitrogen-containing solvents, glycerol fatty acid esters such as mono-, di- and triglycerides and a cetylated mono- and di-glycerides; propylene glycol esters, ethylene glycol esters, glycerol, cholic acid or derivatives thereof, lecithins, alcohols and glycine or taurine conjugates, ursodeoxycholic acid, sodium cholate, sodium deoxycholate, sodium taurocholate, sodium glycocholate, N-Hexadecyl-N, N-dimethyl-3-ammonio-1-propanesulfonate, anionic (alkyl-arylsulphonates) monovalent surfactants, palmitoyl lysophosphatidyl-L-serine, lysophospholipids (e.g. l-acyl-sn-glycero-3-phosphate esters of ethanolamine, choline, serine or threonine), alkyl, alkoxyl (alkyl ester), alkoxy (alkyl ether)- derivatives of lysophosphatidyl and phosphatidylcholines, e.g. lauroyl and myristoyl derivatives of lysophosphatidylcholine, dipalmitoylphosphatidylcholine, and modifications of the polar head group, that is cholines, ethanolamines, phosphatidic acid, serines, threonines, glycerol, inositol, and the postively charged DODAC, DOTMA, DCP, BISHOP, lysophosphatidylserine and lysophosphatidylthreonine, zwitterionic surfactants (e.g. N-alkyl-N, N-dimethylammonio-1 -propanesulfonates, 3-cholamido-l-propyldimethylammonio-l -propanesulfonate, dodecylphosphocholine, myristoyl lysophosphatidylcholine, hen egg lysolecithin), cationic surfactants (quarternary ammonium bases), fusidic acid derivatives-(e.g. sodium tauro-dihydrofusidate etc.), long-chain falty acids and salts thereof C2-C6 (eg. oleic acid and caprylic acid), acylcarnitines and derivatives, N-a-acylated derivatives of lysine, arginine or histidine, or side-chain acylated derivatives of lysine or arginine, N-a-acylated derivatives of dipeptides comprising any combination of lysine, arginine or histidine and a neutral or acidic amino acid, N-a-acylated derivative of a tripeptide comprising any combination of a neutral amino acid and two charged amino acids, or the surfactant may be selected from the group of imidazoline derivatives, or mixtures thereof. Each one of these specific surface-active agent constitutes an alternative embodiment of the invention.

Solubilizers referred above include polyvinylpyrrolidone, copolymers of polyvinylpyrrolidone, sugar alcohols like isomalt, sorbitol, xylitol or mannitol, cellulose derivatives (especially hydroxypropylmethyl cellulose (HPMC) and/or hydroxypropyl cellulose (HPC)), cyclodextrines and its derivatives, polyethoxylated castor oil (Cremophor) and combinations thereof. Preferably polyvinylpyrrolidone and copolymers of polyvinylpyrrolidone.

Anti-tacking agent referred above include talc, titanium dioxide, Colloidal silicon dioxide (Aerosil) and combinations thereof. Preferably Colloidal silicon dioxide (Aerosil).

Sweetners used in the present invention are selected from the group consisting of saccharin, sucrose, saccharin sodium, aspartame, potassium acesulfame, sucralose, neotame (not used in beverages), alitame, cyclamate, tagatose and trehalose.

Flavouring agent referred above include D-limonene, thymol, vanillin, carvacrol, cinnamaldehyde, octanoic acid, heptanoic acid, diallyl disulfide, camphor, l-limonene, rosmarinic acid, p- cymene, ?-terpinene, a-pinene, a~thujone and 1,8- cineole; and - at least one organic acid chosen from the group comprising lactic acid, malic acid, benzoic acid, fumaric acid and sorbic acid or an alkali or alkaline earth metal salt thereof.

Solvents used in the compositions of the present invention organic or inorganic solvent or mixtures thereof selected from isopropyl alcohol (IPA), acetone, ethanol, dichloromethane, water and mixtures thereof.

The powders prepared as per the present invention can be further formulated into final dosage forms, but not limited to a capsule, a cachet, a pill, a tablet, a powder, a granule, a pellet, a bead, a particle, a gum, a troche, a lozenge, a pastille, a solution, an elixir, a syrup, a tincture, a suspension, an emulsion, a mouthwash, a spray, a drop, an ointment, a cream, a gel, a paste, a transdermal patch, a suppository, a pessary, a foam, a food product, and combinations thereof.

Another, embodiment of the present invention provides an equipment for the sprouting of fenugreek seeds which is shown in figure 1.

Description of the Sprouting device
Sprouting device developed to speed up the process of germination with controlled hygienic conditions. That is one kind of cylindrical vessels made-up by stainless steel (Food grade). The weight of the different sprouting devices in the ranging of 30 kg to 700 kg. Sprouting device is fully controlled for the maintaining environmental condition as per according to the seed growth. Pressure gauge, oxygen meter, carbon dioxide, temperature meter has been built for the detection & maintaining of internal environmental conditions. Internal assembly of the device contained with perforated racks to place the seed. The device is able to maintained pressure up to 500 PSI. Sterilized air used to build the pressure inside the device. Heating elements with auto cut thermostat fabricated inside the device in order to maintain the sufficient temperature for enhancing the germination process.

The present invention is illustrated in detail but not limiting to, the following examples. It will be apparent to those skilled in the art that many modifications, both to materials and methods, may be practiced without departing from the scope of the invention

Examples 1
S.No Excipients Quantity per tablet (w/w)
A) Fenugreek Powder Granulation Part
1. Fenugreek Powder 10 %-99%
2. Polyethylene Glycol 6000 IP (SINOPOL PEG6000-PD90) 1%-40%
3. Purified Water Q.S.
B) Lubrication and Blending
4. Dibasic Calcium Phosphate (anhydrous) IP (A-Tab) 1% - 20%
5. Sodium Starch Glycollate IP-Type-A (Exposol) 0.1% - 10%
6. Colloidal Silicon dioxide IP (Aerosil N20 Pharma ) 0.1% - 10%
7. Magnesium Stearate IP (TABLUBE Harmonised) 0.1% - 10%
C) Film coating
8. Opadry II Yellow 85F510117 Q.S
9. Purified Water Q.S

Manufacturing process
Dispensing
? Dispense all the raw materials in required quantity.
Sifting
? Sift Fenugreek Powder through #30 sieve using vibratory sifter and collect in polybag.
Binder Preparation
? Dissolve Polyethylene Glycol 6000 in Purified Water under mechanical stirring until clear solution is formed.
Granulation
? Transfer Fenugreek powder into rapid mixer granulator.
? Add complete binder solution at slow rate into dry mix at slow impeller speed and chopper off setting and chopper off setting. Additionally, if required mix the granules for approximately at slow impeller and chopper speed to get desired consistency of granules
Drying
? Dry the wet granules at inlet temperature 45°C in FBD. Rake the granules.
? Check the LOD of the granules once LOD reached up to 6-7 % w/w remove the semi-dried granule from FDB and wet mill the granules.
Wet Milling
? Mill the wet granules through 2 mm screen at 2100 RPM (Knive reverse setting) using Multi Mill.
Drying
? Continue the drying at inlet temperature 45°C in FBD to achieve the target LOD approximately 3.0 to 4.0 % w/w. (Limit: NMT 5.0 % w/w).
Sifting and Milling
? Check the # 30 sieve for physical integrity before and after use.
? Mill the dried granules using multi mill at 2100 RPM (Knive reverse setting) through 1 mm screen.
? Sift milled granules through # 30 sieve using vibratory sifter.
? Mill the retained granules by using multi mill at 2100 RPM (Knive reverse setting) through 1 mm screen and collect in polybag.
? Sift milled granules through # 30 sieve using vibratory sifter.
Dried granules and extra granular material to be taken for blending
? If yield is less than 98% of the dried granules, then calculate the extra granular materials according to the corresponding yield.
? If the yield of dried granules is more than or equal to 98.0%, dispense the theoretical quantity of extra granular materials.
Sifting of Extra Granular Materials
? Check the # 40 sieve and # 60 sieve for physical integrity before and after use.
? Co-Sift dibasic calcium Phosphate IP (A-Tab), Sodium Starch Glycollate IP (Type A) and Colloidal Silicon Dioxide IP through # 40 sieve using vibratory sifter and collect in polybag.
? Sift Magnesium Stearate IP through # 60 sieve using vibratory sifter and collect in polybag.
Blending
? Load the dried granules into blender, Add sifted material and mix for 10 minutes at 15 RPM.
? Load the dried granules into blender, Add sifted material and mix for 10 minutes at 15 RP
Lubrication
? Add sifted material and mix for 5 minutes at 15 RPM.
Compression
? Compress the lubricated blend using Bi-layer compression machine with the following in-process control checks.

Example 2
Exemplary capsule composition

S.No Excipients Quantity per tablet (w/w)
A) Fenugreek Powder Granulation Part
1. Fenugreek Powder 10 %-99%
2. Polyethylene Glycol 6000 IP (SINOPOL PEG6000-PD90) 1%-40%
3. Purified Water Q.S.
B) Lubrication and Blending
4. Dibasic Calcium Phosphate (anhydrous) IP (A-Tab) 1% - 20%
5. Sodium Starch Glycollate IP-Type-A (Exposol) 0.1% - 10%
6. Colloidal Silicon dioxide IP (Aerosil N20 Pharma ) 0.1% - 10%
7. Magnesium Stearate IP (TABLUBE Harmonised) 0.1% - 10%
Filling into capsule shell

Manufacturing process
Dispensing
? Dispense all the raw materials in required quantity.
Sifting
? Sift Fenugreek Powder through #30 sieve using vibratory sifter and collect in polybag.
Binder Preparation
? Dissolve Polyethylene Glycol 6000 in Purified Water under mechanical stirring until clear solution is formed.
Granulation
? Transfer Fenugreek powder into rapid mixer granulator.
? Add complete binder solution at slow rate into dry mix at slow impeller speed and chopper off setting and chopper off setting. Additionally, if required mix the granules for approximately at slow impeller and chopper speed to get desired consistency of granules
Drying
? Dry the wet granules at inlet temperature 45°C in FBD. Rake the granules.
? Check the LOD of the granules once LOD reached up to 6-7 % w/w remove the semi-dried granule from FDB and wet mill the granules.
Wet Milling
? Mill the wet granules through 2 mm screen at 2100 RPM (Knive reverse setting) using Multi Mill.
Drying
? Continue the drying at inlet temperature 45°C in FBD to achieve the target LOD approximately 3.0 to 4.0 % w/w. (Limit: NMT 5.0 % w/w).
Sifting and Milling
? Check the # 30 sieve for physical integrity before and after use.
? Mill the dried granules using multi mill at 2100 RPM (Knive reverse setting) through 1 mm screen.
? Sift milled granules through # 30 sieve using vibratory sifter.
? Mill the retained granules by using multi mill at 2100 RPM (Knive reverse setting) through 1 mm screen and collect in polybag.
? Sift milled granules through # 30 sieve using vibratory sifter.
Dried granules and extra granular material to be taken for blending
? If yield is less than 98% of the dried granules, then calculate the extra granular materials according to the corresponding yield.
? If the yield of dried granules is more than or equal to 98.0%, dispense the theoretical quantity of extra granular materials.
Sifting of Extra Granular Materials
? Check the # 40 sieve and # 60 sieve for physical integrity before and after use.
? Co-Sift dibasic calcium Phosphate IP (A-Tab), Sodium Starch Glycollate IP (Type A) and Colloidal Silicon Dioxide IP through # 40 sieve using vibratory sifter and collect in polybag.
? Sift Magnesium Stearate IP through # 60 sieve using vibratory sifter and collect in polybag.
Blending
? Load the dried granules into blender, Add sifted material and mix for 10 minutes at 15 RPM.
? Load the dried granules into blender, Add sifted material and mix for 10 minutes at 15 RP
Lubrication
? Add sifted material and mix for 5 minutes at 15 RPM.
Capsule filling
? Fill above blend into capsule.

Example 3
Exemplary syrup composition
The syrup composition of the present invention comprising fenugreek powder having the following formulation
S.No Ingredients Quantity (w/v)
1. Fenugreek Powder 5 -50%
2. Propylene glycol 10 - 60%
3. Polyvinylpyrrolidone K-30 1 – 10%
4. Sucrose 10 – 60%
5. Saccharin sodium 01 -10%
6. Sodium benzoate 01 -10%
7. Purified water qs
Total volume 100 ml

Manufacturing process
Fenugreek Powder was added to propylene glycol and of polyethylene glycol to obtain a solution.
Separately, sucrose, saccharin sodium, polyvinylpyrrolidone, Sodium benzoate and orange essence were added to purified water to obtain a solution.
These solutions were mixed to obtain the syrup composition of the present invention comprising Fenugreek.
,CLAIMS:We Claim:
1. Fenugreek powder composition with high trigonelline, saponin, 4-hydroxyisoleucine, galactomannans contents.

2. Fenugreek powder composition as claimed in claim 1, wherein the powder can be formulated into tablet, capsule and syrup using one or more pharmaceutically acceptable excipients.

3. Fenugreek powder composition as claimed in claim 2, wherein pharmaceutically acceptable excipients used herein selected from binders, diluents, fillers, disintegrants, lubricants, flavouring agents, solubilizers, stabilizers, sweeteners and preservatives.

4. Fenugreek powder composition as claimed in claim 2, wherein excipients selected from polyethylene glycol, dibasic calcium phosphate, sodium starch glycollate, colloidal silicon dioxide, magnesium stearate, polyvinylpyrrolidone, sucrose, saccharin sodium and sodium benzoate.

5. Novel process for the preparation of fenugreek powder with high trigonelline, saponin, 4-hydroxyisoleucine, galactomannans contents, wherein the process comprising steps of raw seed optimization, seed treatment, soaking of seed in water, incubation in growth chamber, termination of seed growth and powder preparation.

6. The process for the preparation of fenugreek powder as claimed in claim 5, wherein the process comprising the steps of:
(a) collecting fenugreek seeds from different regions,
(b) treating seeds with surfactants to decrease the microbial load from the fenugreek seeds and accelerate the germination process,
(c) soaking treated seeds in Reverse Osmosis water & ground water at -5 PSI to 50 PSI up to the 4Hrs to 24 Hrs with various temperature range from 20 – 50 degree,
(d) incubating soaked seeds upto 12 days,
(e) sampling germinated seeds from day 1 to day 12 and evaluating for trigonelline, saponin, 4-hydroxyisoleucine, galactomannans content,
(f) terminating the seed growth after 12 days, and
(g) preparing the dry powder from raw sprout material.

7. Novel process for the preparation of fenugreek tablet, fenugreek capsule and fenugreek syrup with high trigonelline, saponin, 4-hydroxyisoleucine, galactomannans content using fenugreek powder.

8. The process for the preparation of fenugreek tablet as claimed in claim 7, wherein the process comprising the steps of:
(a) sifting the fenugreek powder through sieve,
(b) preparing the binder solution by dissolving binder in purified water,
(c) granulating the fenugreek powder with above binder solution,
(d) milling and drying the granules,
(e) adding extra-granular excipients to the above granules,
(f) compressing the granules into tablets, and
(g) optionally, coating the tablets with film coating or sugar coating.

9. The process for the preparation of fenugreek capsule as claimed in claim 7, wherein the process comprising the steps of:
(a) sifting fenugreek powder through sieve,
(b) dissolving the binder in purified water to make binder solution,
(c) granulating the fenugreek powder using above binder solution,
(d) milling and drying the granules,
(e) adding extra-granular excipients to the above granules and mixing, and
(f) filling the granules into capsules.

10. The process for the preparation of fenugreek syrup as claimed in claim 7, wherein the process comprising the steps of:
(a) adding the fenugreek powder to the carriers to obtain a solution,
(b) adding sweeteners, solubilizers, preservatives and flavouring agents to the water to obtain a solution, and
(c) mixing these solutions to obtain the syrup.

Date this Eighth (08th) day of March, 2019

__________________________________
Dr. S. Padmaja
Agent for the Applicant
IN/PA/883