Title of Invention

"A NOVEL PROCESS FOR THE PRODUCTION OF OLEORESIN FROM FRESH GREEN CHILLI"

Abstract

'The present invention relates to a novel process for the production of oleoresin directly from fresh green chilli (Capsicum \ L. ). This invention leads to the production of an oleoresin conforming to the quality characteristics of the product now being produced commercially from dried ripe chilli with reference to its pungency. The product has the additional advantage of having the characteristic green chilli flavour. High pungent green chilli powder is a useful byproduct in the process,

Full Text

The present invention relates to a novel process for the production of oleoresin directly from fresh green chilli (Capsicum anmiurn L. ). This invention leads to the production of an oleoresin conforming to the quality characteristics of the product now being produced commercially from dried ripe chilli with reference to its pungency. The product has the additional advantage of having the characteristic green chilli flavour. High pungent green chilli powder is a useful byproduct in the process. Chilli oleoresin is mainly valued for its pungency which consists of capsaicin and its allied compounds. Capsaicin, the major pungent principle with the structure, 8-methyl-6-nonenoyl vanillylamide, alongwith dihydrocapsaicin, nor-hydrocapsaicin, homocapsaicin and homo dihydrocapsaicin are collectively referred to as capsaicinoids, Capsaicin finds application in several pharmaceutical preparations especially in pain balms,counter irritants etc. The bulk of the crop is usually prepared for the market by drying of the red ripe chilli pods in the sun. Drying takes about 10 days and pungency is lost to the extent of 15-20%.Capsaicin is sublimable and hence its loss depends on post-harvest conditions of chilli including drying. In the present invention, fresh green chilli is the starting material, drying step is avoided and original flavour quality is retained in the final product. This novel process thus facilitates the direct processing of the freshly harvested produce in growing region. The spoilage of the produce under unfavorable climatic conditions and problems of transportation of the fresh material in bulk to drying centres can be overcome and growers can get better returns for their crop. The final product of green chilli oleoresin can be used for flavoring all types of processed foods where the fresh green chilli flavour is preferred to that of dried chilli. The characteristic green chilli flavour is appreciated in preparations such as chutneys, soups, salads and certain special food preparations. The alkyi methoxy pyrazines are reported to be the highly potent aroma compounds in green chilli. The 2 -methoxy 3-isobutyl pyrazine, limonene, trans-beta-ocimene, methyl salicylate and linalool are found to be the major characteristic fresh aroma constituents. Other significant aroma compounds of green chilli are the C9 and C7unsaturated ketones. Capsaicin content and the original fresh flavour quality are taken care of in this novel process. The volatiles of fresh chilli which are highly heat-sensitive compounds are generally isolated by vacuum distillation-continuous solvent extraction method. Odour-significant compounds were separated by preparative GC on packed columns and re-purified for identification. The major character- impact component was identified as 2-methoxy 3-isobutyl- pyrazine and it has been found to have one of the lowest odour thresholds. Other odour-impact compounds are the C9 unsaturated ketones , nona- and deca dienals and a few terpenic compounds. [Buttery,R.G., Seifert, R.M., Guadagni,D.G.,and Ling,L.C., Charaterisation of some volatile constituents of bell peppers. /. Agric, Food Chem.,17,1322,(1969)J. Another similar study reported the isolation and identification of odour compounds from fresh green mature fruits of three cultivars of Capsicum annuum. Nine odour significant compounds were identified. [Chitwood,R.L.,Pangborn,R.,M.,and Jennmgs,W.,GC-MS and Sensory analysis of volatiles from three cultivars of Capsicum, Food Chem.,11, 201,(1983)]. The unique flavour characteristics of fresh chilli have already been established thus through detailed studies. These flavour constituents which are highly heat-sensitive are almost completely lost during drying. Since fresh chilli is the starting material in this novel process original flavour characteristics are retained in the oleoresin. Recovery of capsaicin (pungency) or its enrichment in oleoresin is essentially based on extraction of ground dried chilli with permitted solvents followed by fractionation using selective reagents for capsaicin. Extraction method of capsaicin is reported from lyophilised fresh green chilli and very high yields are reported compared to extractions from dried chilli [Neil LSass, Mark Rounsavill and Harold Combs., A High- yield Method for the Extraction and Purification of Capsaicin, J. Agric. Food Chem.,25(6),1419-20 (1977)]. Thus fresh green chilli oleoresin by this novel process is the ideal starting material for the best recovery of capsaicin. No process is known in commerce now for the production of oleoresin directly from fresh green chilli. Presently available chilli oleoresin product is prepared from dried chilli. There are no reports on earlier attempts for direct processing of fresh chilli. Very high moisture content in fresh chilli may pose technological problems in direct extraction of fresh chilli and result in poor extraction efficiency. Capsaicin enrichment in the oleoresin or isolation of capsaicin are generally tried from the oleoresin prepared from dried chilli. . The main objective of the present invention is to provide a novel process for the production of oleoresin from fresh chilli which obviates the drawbacks as detailed above. Another objective of the present invention is to provide a method for obtaining an ideal starting material for capsaicin enrichment in the oleoresin or its isolation. Another objective of the present invention is to provide a method for obtaining green chilli powder with capsaicin content in the range that is normally specified for chilli. Accordingly the present invention provides a process for the production of oleoresin from fresh green chilli which comprises crushing of the cleaned chilli to a paste -like consistency in a suitable mill, substantial dewatering of the chilli paste by pressure techniques to get aqueous phase and solid cake, separating the solid from aqueous phase by centrifugation and/or filtration and extracting the combined sediment and the solid cake using permitted organic solvents, followed by desolventisation to get the oleoresin. The solubility characteristics of capsaicin in water is also advantagiously made use of in its preferential retention to the solid portion. Dewatering is the most crucial step in the process and the degree of water removal from the fresh material determines to a large extent the overall efficiency of the process. The oleoresin obtained in this process may be used as the starting material for enrichment or isolation of capsaicin by solvent extraction or adsorption techniques. In an embodiment of the present invention, green chilli paste may be prepared by hammer mill or grinder mixer. In another embodiment of the present invention, dewatering of chilli paste may be carried out by hand press, screw press or hydraulic press. In yet another embodiment of the present invention, the aqueous phase may be subjected to high speed centrifugation or filtration whereby the solid portion is separated and combined with the solid cake obtained by pressing . In yet another embodiment of the present invention the combined solid portion may be directly extracted using permitted solvents viz. ethyl alcohol, dichloroethane or acetone for the oleoresin. The following procedure has been developed for the processing of fresh chilli (Capsicum annuum.L) to get oleoresin as the main product. Freshly harvested chilli pods are cleaned in a washing tank and the cleaned spice is subjected to size reduction and reduced to a paste form using a hammer mill. Alternatively, an ordinary grinder mixer or pinmill are also used for making the paste. The paste is then manually fed into the screw press for dewatering. Alternatively hydraulic press and simple hand press are also used in different experiments. Fresh chilli contains 80-85% moisture. In the dewatering step the compression ratio is so adjusted that about 75-80% of the total moisture is removed from the material. For more effective water removal, pressing is tried in two steps in different experiments. Equal weight of water is added to the residue obtained in the first pressing, mixed well and again subjected to pressing. The juice obtained in the first and second pressing are combined together to have the total aqueous portion. Separation of solid and liquid phases of the aqueous portion is effected by centrifugation and/or filtration in different experiments. The residue obtained in the dewatering step and the solid separated from the aqueous portion are combined together and extracted for oleoresin in the wet condition itself using solvents viz. acetone, ethylene dichloride, ethyl acetate and hexane-acetone mixture . Solid- solvent ratios of 1:5 and 1:6 are used in extraction. The extract is desolventised by distillation under vacuum followed by removing the traces of solvent in a thin- film evaporator to get the oleoresin. Selective solvent extraction is the known effective method for preparation of capsaicin- enriched oleoresin. An overall recovery of 85-90% is realized for capsaicin in the process based on the total capsaicin available in the fresh spice. The moisture content in the original spice and in products at different stages of processing are estimated by Dean - Stark apparatus and capsaicin by BIS method. There are no reports on earlier attempts of processing fresh chilli commercially for its oleoresin. In the novel process, fresh chilli is first dewatered during which step 75-80% of water present in the spice is removed and pungency (capsaicin) is distributed between the solid and liquid phases obtained during the dewatering step. The distribution ratio of capsaicin between the solid and liquid phases is approximately in the ratio of 5:1. The exact distribution ratio will depend on the capsaicin content of the raw material (chilli) used in each experiment. The aqueous portion is subjected to high speed centrifugation and the wet sediment is thoroughly mixed with the solid portion from the dewatering step. The total solid is extracted using permitted solvents such as ethylene dichloride, acetone, ethyl acetate and hexane-acetone mixture. The extract is desolventised by known methods to get the oleoresin. The oleoresin obtained conforms to specifications of the commercial chilli oleoresin with respect to its capsaicin content. The oleoresin thus obtained can be directly marketed as such and/or suitably processed for capsaicin enrichment by known methods of selective solvent extraction. The products have great potential for export-market. The following examples are given by way of illustration and therefore should not be construed to limit the scope of the present invention. Example 1 50 kgs of fresh chilli pods of 84% moisture content were cleaned in washing tank and then subjected to size reduction and made into a paste form using a grinder. The paste was fed into the hydraulic press for dewatering and 77% of the total moisture was removed in this step. Capsaicin was distributed between the solid and liquid phases in the ratio 5:1.5. The moisture content in the original spice and at different stages of processing were estimated by Dean-stark apparatus and capsaicin content was estimated by BIS method. The aqueous layer (37.4kgs) was subjected to high speed centrifugation and the wet sediment (4.2kgs) was mixed thoroughly with the wet solid cake (10.7kgs) .The total solid was used for oleoresin preparation by solvent extraction method. The solvent used was ethyl acetate and solid to solvent ratio of 1:5 was used for extraction. The solvent extract was desolventised by the method described under the general process steps. Overall recovery of capsaicin was 86% based on the original content of capsaicin in fresh chilli. Example 2 30 kgs of fresh chilli pods of 83% moisture content, after cleaning, was subjected to size reduction and made into a paste form using a pin mill, The paste was fed into the screw press for dewatering and 79% of the total moisture was removed in this step. Capsaicin was distributed between the solid and liquid phases in the ratio 5.5:1.5 The moisture content in the original spice and at different stages of processing was estimated by Dean- stark apparatus and capsaicin content was extracted by BIS method. The aqueous layer (20.5 kg) was subjected to high speed centrifiigation and the wet sediment (2 kg) was mixed thoroughly with the solid portion (7.8 kg) .The total solid was used for oleoresin preparation by solvent extraction method. The solvent used was ethylene dichloride and solid to solvent ratio of 1:6 was used for extraction. The solvent extract was desolventised by the method described under the general process steps. Overall recovery of capsaicin was 88% based on the original content of capsaicin in fresh chillies. Example 3 40 kgs of fresh chilli pods of 82% of moisture content were cleaned in a washing tank and the cleaned chilli was subjected to size reduction in a hammer mill. The paste was fed into a hand press for dewatering and 78% of the total moisture was removed in this step. Capsaicin was distributed between the solid and liquid phases in the ratio 5:0: 1.2. The moisture content in the original spice and at different stages of processing were estimated by Dean-Stark apparatus and capsaicin content was estimated by BIS method. The aqueous layer (26.8 kg) was subjected to high speed centrifugation and the wet sediment (2.8 kg) was mixed thoroughly with the solid portions (11 kg) The total solid was used for oleoresin preparations by solvent extraction method. Acetone was used as the extraction solvent and solid to solvent ratio of 1:6 was used for extraction,. The solvent extract was desolventised by the method described under the general process steps. Overall recovery of capsaicin was 87% based on the original content of capsaicin in fresh chilli. The main advantages of the present invention are: 1. The novel technique is cost effective for processing fresh chilli into value added products of oleoresin and capsaicin. 2. The pungency (capsaicin) content of the oleoresin obtained from fresh chilli is always on the higher side compared to the corresponding product from the dried sample. Loss in capsaicin contact during drying is avoided since fresh chilli is directly processed for its value added products. 3. Product of oleoresin from fresh chilli by this invention conforms to the quality specifications of its commercial counterpart with respect to capsaicin content which is prepared from dried chilli. 4. Oleoresin product obtained by this invention has characteristic green chilli flavour and can be used in food preparations where ever green chilli flavour is preferred. 5. Green chilli powder is another useful product in this process which may be used in food preparations where ever green chilli with its special flavour and colour is preferred. We claim: 1. A novel process for the production of oleoresin from fresh green chilli pods [Capsicum annuum L.] which comprises: [a] size reduction and crushing of cleaned chilli to a paste-like consistency; [b] dewatering of the chilli paste obtained in step [a] by applying pressure techniques such as herein described to obtain aqueous portion and solid cake; [c] separating the solid from the aqueous portion as obtained in step [b] by filtration or centrifugation to obtain a sediment; [d] extracting the combined sediment of step [c] and solid cake of step [b] using permitted organic solvents of the kind such as herein described followed by desolventisation to obtain the desired oleoresin. 2. A process as claimed in claim 1, wherein the size reduction of chilli is effected by grinding or crushing in a suitable mill or grinder. 3. A process as claimed in claim 1, wherein dewatering of chilli paste is done either by hydraulic press, screw press or any other pressing machine. 4. A process as claimed in claim 1, wherein the solvent extraction is effected using solvents namely ethylene dichloride, acetone or acetone-hexane mixture with solids solvents ratio in the range of 1 : 5 to 1 : 6. 5. A novel process for the production of oleoresin from fresh green chilli pods substantially as herein described with reference to the foregoing examples.

Documents:

196-del-2003-abstract.pdf

196-del-2003-claims-(11-11-2008).pdf

196-del-2003-claims.pdf

196-del-2003-correspondence-others-(11-11-2008).pdf

196-del-2003-correspondence-others.pdf

196-del-2003-correspondence-po.pdf

196-del-2003-description (complete).pdf

196-del-2003-form-1-(11-11-2008).pdf

196-del-2003-form-1.pdf

196-del-2003-form-18.pdf

196-del-2003-form-2.pdf

196-del-2003-form-3.pdf