JP2007527359A - Non-thermal treatment method for concentrating Garcinia extract - Google Patents

Abstract

The present invention relates to a non-thermal process for obtaining a concentrated garcinia extract using osmotic membrane distillation (OMD).

Description

  The present invention relates to a non-thermal process for concentrating a Garcinia extract. The invention particularly relates to a method for obtaining concentrated Garcinia extract using osmotic membrane distillation (OMD).

  As a dietary supplement, (-)-hydroxycitric acid (HCA) is an effective substance for any weight management program. Allison et al. Is considering the use of HCA as an alternative to weight loss therapy (Crit. Rev. Food Sci. Nutr. 2001, 41, 1-28). Derivatives of HCA are included in many pharmaceuticals in combination with other ingredients for the purpose of promoting weight loss, promoting cardioprotection, promoting dyslipidemia and enhancing endurance (Jena et al., 2002, J. Agric. Food Chemistry, 50, 10-22). To date, HCAs have been identified in certain genus of Garcinia, including G. cambogia, G. indica, G. atroviridis, and G. cowa. It has been found in seed fruits (Lewis, YS 1969, Methods in enzymology, 13, 613-623; Jena et al., 2002, J. Agric. Food Chemistry, 50, 10-22). Recently, the chemistry and biochemistry of HCA has been discussed (Jena et al., 2002, J. Agric. Food Chemistry, 50, 10-22). As a result of extensive animal experiments, HCA has proven to effectively suppress appetite, inhibit food intake, promote hepatic glycogen synthesis, reduce fatty acid synthesis and lipogenesis, and reduce weight gain.

  The genus Garcinia (Hyperaceae) is a large genus of polygamous trees or shrubs distributed in tropical Asia, Africa and Polynesia. The genus Garcinia consists of 180 species, of which about 30 are found in India. Garcinia pedunculata and Garcinia Kowa grow in northeastern India and the Andaman Islands. In Assam, Garcinia Kowa is often grown by farmers because of its sour fruit (The Wealth of India, 1956). The fruits of these two species of the genus Garcinia cannot be said to be good because of their strong acidity. In the Assam region, fruit slices dried in the sun are used for cooking and as a folk medicine.

  Reference can be made to commercial samples of Garcinia Cambodian extracts containing calcium salts of HCA (Sawada, et al, 1997, Nihon yukagaka kaishi, vol 1467-1474). However, when calcium is excessive, solubility and bioavailability are reduced compared to liquid extracts.

  Reference may also be made to US Pat. No. 656314 (Ashok kumar., Ravindranath, B., and Balasubramamanvam, 1996). This method includes water extraction, subsequent flow through an ion exchange resin and decolorization using activated carbon, and final concentration using vacuum evaporation. The main drawbacks of this method are that it is a thermal process and that many unit operations are performed before obtaining the final product.

  In addition, a method for preparing potassium hydroxycitrate from fruits of the genus Garcinia has been reported and can be referred to (Majeed, M., Badmaev, V and Rajendran, R., US Pat. No. 5,783,603, 1998). This method involves the extraction of Garcinia fruit with an alkyl alcohol, the extract being treated with potassium hydroxide and then refluxed to produce a precipitate of potassium hydroxycitrate. The main drawback of this method is that the potassium salt is hygroscopic. In addition, since the natural state of HCA cannot be used, bioavailability and versatile use for pharmaceutical purposes are limited.

  It is noted that all these references are reports on the preparation of HCA derivatives. However, there is no report of a non-thermal process for concentrating HCA, and there is no report of a non-thermal process for concentrating natural (non-derivative) HCA.

  The main object of the present invention is to develop a process for preparing a liquid concentrated garcinia extract from Garcinia pedunclata / garcinia kowa.

  Another object of the present invention is to develop a non-thermal process for concentrating the extract.

  Yet another object of the present invention is to develop a method for concentrating Garcinia extract using osmotic membrane distillation (OMD).

  Yet another object of the present invention is to provide a simple one-step and efficient and economical method for enriching native form of HCA.

Therefore, the present invention
a) collecting dried fruit hulls originating from Garcinia spp.
b) Manually cutting the outer skin of Garcinia pedunkurata / garcinia kowa to a size of 3 × 9 mm to 6 × 14 mm,
c) extraction with deionized water at a volume ratio of 1: 4 at 110-130 ° C. for 15-35 minutes,
d) filtering the extract with a filter cloth;
e) concentrating HCA by performing osmotic membrane distillation (OMD) in a co-current flat membrane module;
f) placing a hydrophobic membrane between two steel frames SS316 with the appropriate space of the module;
g) circulating the extract at a flow rate of 100-150 ml / min on one side of the membrane using a multistage peristaltic pump;
h) a hydrophobic membrane osmotic agent (OA) on the other side of the membrane using a multistage peristaltic pump;
i) performing OMD for about 4-6 hours until the extract is concentrated in the feed tank;
A non-thermal treatment method for concentrating a Garcinia extract is provided.

  In one embodiment of the present invention, the HCA concentrate is obtained from an aqueous extract of Garcinia peduncrata and Garcinia kowa.

  In another embodiment of the present invention, the concentrated Garcinia extract is subjected to non-thermal membrane treatment methods, ie osmotic membrane distillation (OMD) at room temperature (25 ± 1 ° C.) and ambient pressure (1 atm). To obtain.

  In yet another embodiment of the invention, the HCA content of the concentrated Garcinia extract is in the range of 33-37% as measured by HPLC method.

  In yet another embodiment of the invention, the HCA content is increased 4-6 fold, and HCA is as a natural form (not a derivative) that increases its commercial and nutritional value without producing a lactone. The existing Garcinia extract is concentrated by a simple one-step method.

  In the present invention, the outer skin of Garcinia pedunclata / garcinia kowa was cut into small pieces and extracted with deionized water. The extract was filtered through a filter cloth (filter cloth).

  HCA was concentrated by performing osmotic membrane distillation in a co-current flat membrane module. The membrane module consisted of two steel frames SS316, with a hydrophobic membrane placed between them. Using a multi-stage peristaltic pump, the entire filtrate was circulated on one side of the OMD membrane and osmotic agent (OA) was circulated on the other side. After circulating for the desired time, the extract was concentrated in the feed tank.

The purity of the preparation was analyzed by HPLC method as reported by Jayaprakasha, GK and Sakariah, KK (J. Liquid Chromatography & Related Technologies, 23, 915-923, 2000). Concentrated hydroxycitric acid (0.1 g) was dissolved in water, water was added to 100 ml and filtered. A Hewlett-Packard HPLC model HP1100 equipped with a Waters Microbonder Pack ^TM C ₁₈ column (length 250 mm x inner diameter 4.6 mm: Waters, Milford, Massachusetts, USA) was used for the high performance liquid chromatography system. A series (Hewlett Packard, California, USA) was used. The introduction system (Rheodyne) used a 20 μL sample loop.

  Detection was performed at a wavelength of 210 nm with an HP1100 series variable wavelength detector. Elution was performed using 8 mM sulfuric acid, and the flow rate was 1.0 ml / min under isocratic conditions. A known amount (10 μl) of the sample was introduced into the HPLC and the dilution factor was applied to determine the HCA concentration directly from the peak area. The HCA concentration of the sample was expressed in grams per 100 g of sample (g / 100 g of sample). The purity of hydroxycitric acid was 33 to 35% by weight.

The important features of the present invention are as follows.
1. A concentrated Garcinia extract can be obtained by non-thermal membrane treatment.
2. This method can obtain a concentrated extract in one step.
3. In this method, no phase change occurs.
4). Since the method is performed at room temperature and ambient pressure, the product is not thermally damaged.
5). The HCA content increases 4 to 6 times.
4). In this method, no lactone is produced.

  The following examples are given for illustration of the invention and should not be construed as limiting the scope of the invention.

Example 1
Garcinia Pedunclata's 500g fruit skin was cut into small pieces and extracted with 1.5 liters of deionized water at 120 ° C for 20 minutes. The extract was filtered through a filter cloth. The extract was removed and concentrated by osmotic membrane distillation at a flow rate of 100 ml / min in a co-current flat membrane module using a microporous and hydrophobic 0.05 μm polypropylene membrane. The module was operated in cocurrent mode with saturated calcium chloride as the osmotic material. It was concentrated until the volume of the extract was reduced to 1/5 of the original volume. The concentration of HCA increased from 6 ° Brix (Brix concentration) to 62 ° Brix. When the HCA content was measured by HPLC method, the HCA increased from the initial 5.09% to 33.58% (6-fold increase).

Example 2
Garcinia Kowa fruit skin 1000g was cut into small pieces and extracted with 3 liters of deionized water using autoclave at 130 psi pressure for 30 minutes. The extract was filtered through a filter cloth. The extract was removed and concentrated by osmotic membrane distillation at a flow rate of 130 ml / min in a co-current flat membrane module using a microporous and hydrophobic 0.05 μm polypropylene membrane. The module was operated in cocurrent mode with saturated calcium chloride as the osmotic material. It was concentrated until the volume of the extract was reduced to 1/5 of the original volume. The concentration of HCA increased from 6 ° Brix to 62 ° Brix. When the HCA content was measured by HPLC method, HCA increased from the initial 6% to 35.5% (7-fold increase).

Example 3
Garcinia Pedunclata fruit skin 100g was cut into small pieces and extracted with 1 liter of deionized water at 120 ° C for 50 minutes using an autoclave. The extract was filtered through a filter cloth. The extract was removed and concentrated by osmotic membrane distillation at a flow rate of 150 ml / min in a co-current flat membrane module using a microporous and hydrophobic 0.05 μm polypropylene membrane. The module was operated in cocurrent mode with saturated calcium chloride as the osmotic material. It was concentrated until the volume of the extract was reduced to 1/5 of the original volume. The concentration of HCA increased from 6 ° Brix to 62 ° Brix. When the HCA content was measured by HPLC method, HCA increased from the initial 5% to 34.5% (6-fold increase).

The main advantages of the present invention are as follows.
1. This method is a method capable of obtaining concentrated free HCA in one simple step.
2. This concentrated garcinia extract is a natural type rather than derivatives such as sodium salt, potassium salt and calcium salt. Therefore, this concentrated garcinia extract has better bioavailability.
3. Since the method is non-thermal, the product is not subject to any thermal damage. The product is therefore suitable for food and therapeutic applications.
4). The method can be easily scaled up.

Claims (11)

a) collecting and cutting fruit hulls selected from the species of the genus Garcinia, Garcinia peduncrata and Garcinia kowa;
b) extracting the cut skin with deionized water at 115-130 ° C. for 20-30 minutes at a volume ratio of 1: 4 to obtain an extract;
c) filtering the extract to obtain a particle-free extract;
d) osmotic membrane distillation of the particulate extract in cocurrent mode in the presence of osmotic material until the volume of the extract is reduced to 1/5 of the original volume;
A non-heat treatment method for concentrating a Garcinia extract.   The method of claim 1, further comprising obtaining hydroxycitric acid from the concentrated extract of step (d).   The method according to claim 1, wherein the hydrophobic membrane is arranged between two steel frames SS316 of a module having a suitable space.   The method according to claim 1, wherein the extract is circulated on one side of the membrane at a flow rate of 100 to 150 ml / min using a multistage peristaltic pump.   The method of claim 1, wherein a hydrophobic membrane permeation material (OA) is placed on the other side of the membrane using a multistage peristaltic pump.   The method of claim 1, wherein the osmotic material is saturated calcium chloride.   The method according to claim 1, wherein the osmotic membrane distillation is performed at a room temperature of 25 ± 1 ° C. and a pressure of 1 atmosphere.   The method of claim 1, wherein the osmotic membrane distillation is performed for about 4-6 hours until the extract is concentrated in a feed tank.   The method according to claim 1, wherein the content of the free hydroxycitric acid in the concentrated product is in the range of 33 to 35% as measured by HPLC method.   2. The content of hydroxycitric acid is increased 4 to 6 times, and HCA exists as a natural form (not a derivative) that increases its commercial and nutritional value without producing a lactone. the method of. a) collecting the rind of dried fruits arising from Garcinia sp.
b) manually cutting the outer skin of Garcinia pedunkurata / garcinia kowa to a size of 3 × 9 mm to 6 × 14 mm;
c) extracting with deionized water at a volume ratio of 1: 4 at 110-130 ° C. for 15-35 minutes;
d) filtering the extract through a filter cloth;
e) concentrating HCA by performing osmotic membrane distillation (OMD) in a co-current flat membrane module;
f) placing a hydrophobic membrane between two steel frames SS316 having appropriate space in the module;
g) circulating the extract at a flow rate of 100-150 ml / min on one side of the membrane using a multistage peristaltic pump;
h) a hydrophobic membrane permeate (OA) step on the other side of the membrane using a multi-stage peristaltic pump;
i) performing OMD for about 4-6 hours until the extract is concentrated in the feed tank;
A non-heat treatment method for concentrating a Garcinia extract.