Claims:
We claim:
1) A triple salt composition of hydroxycitric acid from Garcinia species, said triple salt includes magnesium at a concentration ranging from about 11% to about 15 %, calcium and potassium each at a concentration not more than about 3%.
2) The composition as claimed in claim 1, wherein magnesium is preferably at a concentration of about 11.71%, calcium is preferably at a concentration of about 0.13% and potassium is preferably at a concentration of about 0.71%.
3) The composition as claimed in claim 1, further comprising hydroxycitric acid at a concentration ranging from about55% to about 65% andlactone ranging from about 0% to about 0.5%.
4) A process for preparing triple salt composition of hydroxycitric acid from Garcinia species as claimed in claims 1 to 2, wherein said process comprising steps of: (a) preparing an extract from Garcinia Cambogia followed by precipitation to remove the impurities from the extract; (b) obtaining concentrate of the extract followed by decolorizing and neutralizing steps to obtain the extract; and (c) precipitating the neutralized extract to obtain white precipitate followed by diluting, decolorizing and spray drying.
5) The process as claimed in claim 4, wherein the Garcinia Cambogia fruit is extracted with water at a ratio of 1:2 volume of water for a time period of about 3 hours.
6) The process as claimed in claim 4, wherein said precipitation to remove the impurities is carried out using mixture of calcium hydroxide and magnesium hydroxide followed by filtration and concentrated to 25 TSS under vacuum.
7) The process as claimed in claim 6, wherein the concentrate obtained is further decolorized using activated charcoal followed by neutralizing using mixture of magnesium hydroxide and potassium hydroxide.
8) The process as claimed in claim 7, wherein said neutralized extract is precipitated by adjusting pH to 3 followed by concentration to 50 TSS under vacuum.
9) The process as claimed in claim 8, wherein said precipitate concentrate is further precipitated using 80 % methanol at a ratio of 1:2 to obtain a white colored precipitate followed by separating and diluting in water to 30 TSS and decolorizing to obtain a clear liquid which is subjected to spray dried at an inlet temperature of about 1950C and an outlet temperature of about 950C to obtain triple salt of hydroxycitric acid.
10) A formulation comprising the composition as claimed in claims 1 to 2, wherein said formulation type is selected from a group comprising pharmaceutical, beverage and dietary or nutraceutical formulation.

, Description:FORM 2
The Patent Act 1970
(39 of 1970)
&
The Patents Rules, 2003
(See section 10 and rule 13)

Complete Specification

Title: A Composition of HCA and a Process Thereof

Name of the Applicant:
Prakruti Products Private Limited,No. 86, 3rd floor, 22nd main, BSK 2nd Stage, Bangalore – 560070, Karnataka, India

Nationality: Indian

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

Technical Field
The present disclosure relates to triple salt composition of hydroxycitric acid from Garcinia species and a process to prepare such a composition.
Background
The (-)-hydroxycitric acid (HCA) is a naturally occurring acid found in the rinds of the fruit of Garcinia cambogia, Garcinia indica and Garcinia mangostana. A number of patents have been granted for the preparation / isolation of (-)HCA salts. They are used as dietary supplement and food products to reduce body weight. The primary mechanism of action of (-)HCA appears to be related to act as a competitive inhibitor of the enzyme ATP-citrate lyase, which catalyzes the conversion of citrate and coenzyme A to oxaloacetate and acetyl coenzyme A (acetyl-CoA). Extensive experimental studies suggest that (-)HCA suppresses the fatty acid synthesis, lipogenesis and food intake thus leading to weight reduction. In addition to suppression of fatty acid and fat synthesis, (-)HCA is thought to suppress food intake via loss of appetite by stimulation of liver gluconeogenesis. Various researchers have evaluated HCA for its weight control properties, fat burning properties, lipid level lowering effect, appetite regulation, metabolic rate increase and other effects. Reported are various salts of (-)HCA with varying concentrations of salts. But, none of them discloses the triple salt composition of Garcinia species as disclosed in the present disclosure. As we know, the calcium content in the body gives strength to the bones, while magnesium helps in maintaining the elasticity to prevent bone injury. Hence, having them in right concentrations can offer various best results to the subjects in need thereof.
In view of the above aspects, there is a need for the development of improved triple salt composition from Garcinia species with rich therapeutic magnesium concentration in it. The present disclosure provides compositions that have the maximum content of magnesium in the triple salt composition obtained from Garcinia species, which eventually helps in giving elasticity to the bones.
SUMMARY
Accordingly, the present disclosure provides a triple salt composition of hydroxycitric acid from Garcinia species, said triple salt includes magnesium at a concentration ranging from about 11% to about 15 %, calcium and potassium each at a concentration ranging from about 1% to about 3% and is also provided for a “A process for preparing triple salt composition of hydroxycitric acid from Garcinia species, wherein said process comprising steps of: (a) preparing an extract from Garcinia cambogia followed by precipitation to remove the impurities from the extract; (b) obtaining concentrate of the extract followed by decolorizing and neutralizing steps to obtain the extract; and (c) precipitating the neutralized extract to obtain white precipitate followed by diluting, decolorizing and spray drying and is also provided for A formulation comprising the composition, wherein said formulation type is selected from a group comprising pharmaceutical, beverage and dietary or nutraceutical formulation.

BRIEF DESCRIPTION OF ACCOMPANYING DRAWING
Figure: 1 HPLC Chromatogram

DETAILED DESCRIPTION
Before explaining any one embodiment of the present disclosure by way of drawings, experimentation, results, and pertinent procedures, it is to be understood that the disclosure is not limited in its application to the details as explained in below embodiments set forth in the following description or illustrated in the drawings, experimentation and/or results. The disclosure is further capable of other embodiments which can be practiced or carried out in various ways. As such, the language used herein is intended to be given the broadest possible scope and meaning; and the embodiments are meant to be exemplary--not exhaustive. Also, it is to be understood that the phraseology and terminology employed herein is for the purpose of description and should not be regarded as limiting.
The present disclosure is in relation to a triple salt composition of hydroxycitric acid from Garcinia species, said triple salt includes magnesium at a concentration ranging from about 11% to about 15 %, calcium and potassium each at a concentration ranging from about 1% to about 3%.
In one embodiment of the present disclosure, wherein magnesium is preferably at a concentration of about 11.71%, calcium is preferably at a concentration of about 0.13% and potassium is preferably at a concentration of about 0.71%.
In one embodiment of the present disclosure, it providescomposition comprising hydroxycitric acid at a concentration ranging from about 55% to about 65% and lactone ranging from about 0% to about 0.5%.
The present disclosure is in relation to a process for preparing triple salt composition of hydroxycitric acid from Garcinia species as explained in above embodiments, wherein said process comprising steps of: (a) preparing an extract from Garcinia Cambogia followed by precipitation to remove the impurities from the extract; (b) obtaining concentrate of the extract followed by decolorizing and neutralizing steps to obtain the extract; and (c) precipitating the neutralized extract to obtain white precipitate followed by diluting, decolorizing and spray drying.
In one embodiment of the present disclosure, the Garcinia Cambogia fruit is extracted with water at a ratio of 1:2 volume of water for a time period of about 3 hours.
In another embodiment of the present disclosure, said precipitation is to remove the impurities is carried out using mixture of calcium hydroxide and magnesium hydroxide followed by filtration and concentrated to 25 TSS (Total soluble solids) under vacuum.
In yet another embodiment of the present disclosure, the concentrate obtained is further decolorized using activated charcoal followed by neutralizing using mixture of magnesium hydroxide and potassium hydroxide.
In still another embodiment, the neutralized extract is precipitated by adjusting pH to 3 followed by concentration to 50 TSS under vacuum.
In still another embodiment, the precipitate concentrate is further precipitated using 80 % methanol at a ratio of 1:2 to obtain a white colored precipitate.
In still another embodiment, the white colored precipitate is separated and diluted in water to 30 TSS and decolorized to obtain a clear liquid which is subjected to spray dried at an inlet temperature of about 1950C and an outlet temperature of about 950C to obtain triple salt of hydroxycitric acid.
The present disclosure is in relation to a formulation comprising the composition as explained in above embodiments, wherein said formulation type is selected from a group comprising pharmaceutical, beverage and dietary or nutraceutical formulation.

The triple salts of the present disclosure are used as dietary supplement and food supplement to reduce body weight. The calcium content in the body gives strength to the bones. And magnesium helps in maintaining the elasticity to prevent bone injury. This disclosure has replaced the high potassium in the triple of other patentsby magnesium which helps in giving elasticity to the bones.

Additionally, the disclosure is further illustrated by the following examples, which are not to be construed in any way as imposing limitations upon the scope of the present invention. On the contrary, it is to be clearly understood that various other embodiments, modifications, and equivalents thereof, after reading the description herein in conjunction with the drawings and appended claims, may suggest themselves to those skilled in the art without departing from the spirit and scope of the presently disclosed and claimed invention.
Example 1: Extraction of (-) HCA from Garcinia Cambogia fruit rind
In the present processGarcinia Cambogia fruit rind is extracted in water. The extraction process is done by soaking the fruit rind in 1:2 volume of water for 3 hr with continuous stirring. Three successive extractionsare done with 1:2 volume of water for 3 hrs each. The combined extracts of all the three washes is then precipitated using mixture of calcium hydroxide andmagnesium hydroxide to remove the unwanted material from the extract by adjusting the pH to 3 to 3.5. This is then filtered and the filtrate is concentrated to 25 TSS under vacuum. The concentrate obtained is decolorized using activated charcoal. Further the colorless extract is neutralized using the mixture of magnesium hydroxide and potassium hydroxide. The neutralized,colorless extract is further concentrated to 50 TSS under vacuum. It is then precipitated using 80% methanol in the ratio 1:2.The white precipitate formed is filtered and dissolved in water to 30 TSS. The clear liquid is then spray dried at in let temperature of about 190oC and outlet temperature of about 95oC.
Example 2: The triple salt obtained issubjected to various known physical, chemical, microbiological and other tests – the results of the same are captured in below table.

Parameter Specification
Physical
Description White colored powder, hygroscopic in nature.
Odor Characteristic
pH(1% solution) 6.0-9.0
Loss on drying Not more than 8.0% w/w
Loose bulk density 0.2-0.6g/ml
Tapped bulk density 0.5-0.8g/ml
Solubility Soluble in water
Sieve test (passes through)
-40 mesh Not less than 95% w/w

Chemical
Assay of Hydroxy citric acid by HPLC Not less than 60.0% w/w
on dried basis
Content of Magnesium Not less than 8.0% - determined by AA spectroscopy
Content of Calcium Not more than 3.0% - determined by AA spectroscopy
Content of Potassium Not more than 3.0% - determined by AA spectroscopy

Others
Lead Not more than 3.0 ppm – determined by ICP-MS
Arsenic Not more than 1.0 ppm – determined by ICP-MS
Cadmium Not more than 1.0 ppm – determined by ICP-MS
Mercury Not more than 0.1 ppm – determined by ICP-MS

Microbiology
Total aerobic microbial count Not more than 3000 cfu/g
Total yeast and mould count Not more than 100 cfu/g
Escherichia coli Negative/10g
Salmonella sp. Negative/10g
Staphylococcus aureus Negative/10g
Coliforms Negative/10g

Example 3: Determination of content of Hydroxy citric acid by HPLC
Materials Required:
HPLC grade water, HPLC grade Acetonitrile, Orthophosphoric acid (H3PO4) HPLC grade.

Mobile phase A:100% Acetonitrile filtered through 0.45µm membrane filter and degassed
Mobile phase B:0.2% Orthophosphoric acid (H3PO4) in HPLC water filtered through 0.45µm membrane filter and degassed.
Gradient Program:
Sl. No Time (in mins.) B%
1 0.01 100
2 10 100
3 11 0
4 15 0
5 20 100
6 25 100

Column : Kromasil C18, 250 X 4.6mm, 5µm
Flow rate : 1.2 ml per minute
Run time : 25 minutes
Data acquisition time : 25 minutes
Detector wave length : 210 nm.
Injection volume : 20 µl
Diluent : 25% v/v Orthophosphoric acid (H3PO4) in water

Blank Preparation:
Pipette out 5ml of 25% v/v Orthophosphoric acid solution to a 50ml volumetric flask and dilute to volume with HPLC water, mix well.
Standard Preparation:
Accurately weigh 50 mg of Calcium salt of Hydroxy citric acid, working standard and transfer to a 50 ml volumetric flask. Dissolve with 5 ml of 25% v/v Orthophosphoric acid. Cool the sample and make up to the volume with HPLC water. Filter through 0.45µ Nylon syringe filter or membrane filter.
Sample Preparation:
Accurately weigh 50 mg of Calcium salt of Hydroxy citric acid and transfer to a 50 ml volumetric flask. Dissolve with 5 ml of 25% v/v Orthophosphoric acid .Cool the sample and make up to the volume with HPLC water.
Filter through 0.45 µ Nylon syringe filter or membrane filter.
Stabilize the instrument with above mobile phase. Inject 20µl of blank solution followed by 20µl of the standard solution in triplicate injections. Record the chromatograms. % RSD for area of the triplicate injections of the standard should be NMT 2%. % RSD for the retention time area of the triplicate injections of the standard should be NMT 1%. Inject the sample solution and record the area of the corresponding peak in the chromatogram.

Calculations:
% HCA= Area of HCA peak in the sample X Standard weight(mg) X 50 X Purity of the std.
Area of HCA peak in the standard X 50 X Sample weight (mg)

The results of HPLC are documented in the above table. An HPLC chromatogram is enclosed in drawings as Figure: 1.

While various aspects and embodiments have been disclosed herein, other aspects and embodiments will be apparent to those skilled in the art. The various aspects and embodiments disclosed herein are for purposes of illustration and are not intended to be limiting, with the true scope and spirit being indicated by the following claims.

We claim:
1) A triple salt composition of hydroxycitric acid from Garcinia species, said triple salt includes magnesium at a concentration ranging from about 11% to about 15 %, calcium and potassium each at a concentration not more than about 3%.
2) The composition as claimed in claim 1, wherein magnesium is preferably at a concentration of about 11.71%, calcium is preferably at a concentration of about 0.13% and potassium is preferably at a concentration of about 0.71%.
3) The composition as claimed in claim 1, further comprising hydroxycitric acid at a concentration ranging from about55% to about 65% andlactone ranging from about 0% to about 0.5%.
4) A process for preparing triple salt composition of hydroxycitric acid from Garcinia species as claimed in claims 1 to 2, wherein said process comprising steps of: (a) preparing an extract from Garcinia Cambogia followed by precipitation to remove the impurities from the extract; (b) obtaining concentrate of the extract followed by decolorizing and neutralizing steps to obtain the extract; and (c) precipitating the neutralized extract to obtain white precipitate followed by diluting, decolorizing and spray drying.
5) The process as claimed in claim 4, wherein the Garcinia Cambogia fruit is extracted with water at a ratio of 1:2 volume of water for a time period of about 3 hours.
6) The process as claimed in claim 4, wherein said precipitation to remove the impurities is carried out using mixture of calcium hydroxide and magnesium hydroxide followed by filtration and concentrated to 25 TSS under vacuum.
7) The process as claimed in claim 6, wherein the concentrate obtained is further decolorized using activated charcoal followed by neutralizing using mixture of magnesium hydroxide and potassium hydroxide.
8) The process as claimed in claim 7, wherein said neutralized extract is precipitated by adjusting pH to 3 followed by concentration to 50 TSS under vacuum.
9) The process as claimed in claim 8, wherein said precipitate concentrate is further precipitated using 80 % methanol at a ratio of 1:2 to obtain a white colored precipitate followed by separating and diluting in water to 30 TSS and decolorizing to obtain a clear liquid which is subjected to spray dried at an inlet temperature of about 1950C and an outlet temperature of about 950C to obtain triple salt of hydroxycitric acid.
10) A formulation comprising the composition as claimed in claims 1 to 2, wherein said formulation type is selected from a group comprising pharmaceutical, beverage and dietary or nutraceutical formulation.

ABSTRACT
Title: A Composition of HCA and a Process Thereof
The present disclosure provides a triple salt composition of hydroxycitric acid from Garcinia species, said triple salt includes magnesium at a concentration ranging from about 11% to about 15 %, calcium and potassium each at a concentration not more than about 3%. It also provides a process of its preparation and it can be used in weight management and/ or its related conditions.