Title of Invention

A PROCESS FOR THE PREPARATION OF STABLE NATURAL GREEN COLORANT FROM THE SKIN OF FRESH GREEN PAPPER BERRIES.

Abstract The present invention provides a process for the preparation of stable natural green colorant from the skin of fresh green pepper berries. The process comprises the steps of bleaching of fresh green pepper berries in water, removing the skin from the bleached berries mechanically or manually to obtain wet mass of skin, stabilizing the above said wet mass of skin using stabilizing agent such as potassium meta bisulphite and sodium meta bisulphite, alkalizing said stabilized wet mass of skin with an aqueous solution of carbonate and bicarbonate of sodium and potassium, drying the wet mass of skin to obtain dried mass of skin using a mechanical drier and extracting the colorant from the dried mass of skin using non-polar solvent such as hexane, ethyl ether, petroleum ether and polar solvent selected from group consisting of methyl alcohol, acetone and water.
Full Text The present invention relates to a process for the preparation of stable natural green colorant from the skin of fresh green pepper berries.
There is a considerable interest around the world in the development of food colours from natural sources as alternates for synthetic colorants. Natural green colorant has been made using specific raw materials such as alfalfa, spinach, algae, olive skin, palm fibre, kiwi fruit, cereal grasses, carrot tops etc.
In this process, the green pepper berries obtained directly or as a byproduct from the process of making white pepper is stabilised to retain the green colour and the colour is then subsequently extracted.
Chlorophyll, the green pigment of plants, is extracted and widely used as a natural colouring matter in various food items. Patent literature on the preparation of chlorophyll colorants can be classified into categories namely, extraction with organic solvents such as alcohol or acetone, aqueous extraction, production of alkali metal salts of chlorophyll, preparation of oil solutions and stabilisation of chlorophyll.
Reference may be made to USSR Patent No.342,628 (1972) chlorophyll-carotene paste which deals with the preparation of chlorophyll-carotene paste from evergreen plant materials using an organic solvent such as trichloroethylene.
Reference may be made to UK Patent No. 1,358,052 (1971), process for producing edible powders which deals with the preparation of edible powder from green leaves of barley and wheat wherein the extracted green juice is
neutralised to pH 7.2 and spray dried to get an edible powder for use in the preparation of food items like ice cream.
Reference may be made to Japan Patent No. 72,020,473 (1972), preventing discoloration of chlorophyll on heating which deals with the stabilisation of an alcoholic chlorophyll extract from barley leaf and spray drying. The spray dried powder was extracted with ethanol, clarified with sodium bicarbonate , evaporated and diluted with water. The PH of the extract adjusted to 7.2 prevented discolouration on heating.
Reference may be made to Japan Patent No.72,034,718 (1972), stabilized chlorophyll containing food colorant which deals with the preparation of edible chlorophyll colorant suitable for food use. using lauryl sulphate, diamine salts and propylene glycol.
Reference may be made to Japan Patent No. 74,052,826 (1974), preparation of natural chlorophyll, which deals with the preparation of chlorophyll colorant for food use from chopped grass leaves by extraction with acetone, neutralisation with an aqueous alkaline solution and extraction with ether followed by low-pressure distillation.
Reference may be made to Japan Patent No. 80,157,659 (1980) simultaneous extraction of chlorophylls and carotenoids from algae as food-coloring agents ,which deals with the simultaneous extraction and subsequent preparation of chlorophyll and carotenoids from algae using a mixture of hydrophobic and hydrophyllic solvents followed by concentration and drying.
Reference may be made to Japan Patent No. 80,007,702 (1982) green food colorant from vegetables which deals with the preparation of chlorophyll based green colour wherein a green vegetable is soaked in 1% sodium chloride or sodium bicarbonate, frozen ,thawed pressed and subsequently dried.
Reference may be made to French Patent (1976), process for obtaining vegetable extracts from moist vegetable material which deals with the method of making edible oily or fat soluble vegetable extract such as carotene or chlorophyll concentrate from wet vegetable waste such as olive skin, nettles or palm fiber by extraction with an organic solvent with a boiling point less than 60°C and a solubility of 20-40% in water.
Reference may be made to Netherland Patent (1973)y method of preserving vegetables which deals with the stabilisation of the green vegetable such as green peas, sprout or calabrese is carried out by heating the raw vegetable to at least 50°C in an aqueous solution containing 0.01 to 0.1% (w/v) of cationogenic, alkyl-substituted, quaternary, nitrogen compound such as cetylethylmorpholinoethyl sulfonate. This treatment prevents the conversion of chlorophyll to pheophytin.
The main object to the present invention is to develop A process for preparation of natural green colorant from the skin of fresh green pepper berries.
Accordingly the present invention provides a process for the preparation of stable natural green colorant from the green skin of fresh green pepper berries which comprises
(a) blanching of fresh green pepper berries in water at 90-100°C for a period
of 10-30 minutes or heating of fresh green berries at 140°C -210°C
for a period of 10-20 minutes,
(b) removing the skin from the blanched berries or heated berries using
a mechanical device or manually,

(b) stbilising the above said wet mass obtained using a stabiising solution of a
source of sulphur di oxide selected from potassium meta bi sulphite and
sodium meta bi sulphite of concentration ranging between of 0.01 -1 % at
a pH of 3-6,
(c) alkalising of the wet mass with an aqueous solutions of metal salts selected
from carbonate and bicarbonate of sodium or potassium at a pH of 7.5-
11.0,

(d) drying the above stabilized mass obtained by using a mechanical drier at a
temperature ranges between 40-60° C for 6-8 hours ,
(e) extracting the above said dried material using solvent selected from non
polar group consisting of hexane, ethyl ether,pet.ether and polar solvent
selected from the group consisting of methyl alcohol, acetone and water.
(f) removing the solvent at low pressure in the range of 20-27 inches of
mercury to get desired resinous mass rich in green colour,
In an embodiment of the present invention the green colorant obtained has the
following characteristics - - a resinous mass ; deep green colour having
chlorophyll content of 1-1.7% ;
In an embodiment of the present invention wherein the yield of the colorant is
in the order of 0.5% on the basis of fresh green berries,
In an embodiment of the present invention wherein blanching, of fresh green
pepper berries is preferably carried out at 96-98°C for a period of 10-15
minutes.
In an embodiment of the present invention, wherein concentrate of chemical
stabiliser used preferably in the range of 0.05-0.07%,
In an embodiment of the present invention, wherein the pH for the alkalization
is preferably in the range of 7.5-9.0.
In an embodiment of the present invention, wherein the resinous green color obtained is rendered more useful for food application using a medium of edible oil, fat, fatty acid and permitted emulsifiers for imparting a green or yellowish green colour to selected foods.
In an embodiment of the present invention wherein the natural green colorant obtained is stable for a period of 3 months.
The process is described below by way of flow diagramme.
FLOW SHEET OF THE PROCESS
FLOW SHEET 1
GREEN PEPPER BERRIES
WATER BLANCHING UNDER CONTROLLED CONDITIONS DESKINNING WET SKIN
COLOUR STABILISATION BY SULPHUR DIOXIDE
ALKALISATION, WASHING PRESSING
EXTRACTION← STABILISED WET SKIN
DRY DRY SKIN
I
SOLVENT EXTRACTION
DESLOVENTISATION
FLOW SHEET 1ICOLORANT
GREEN PEPPER BERRIES
CONTROLLED DRY HEAT TREATMENT FOR CHLOROPHYLL STABILISATION
DESKINNING WET SKIN

COLOUR STABILISATION BY SULPHUR DIOXIDE
ALKALISATION, WASHING PRESSING ↓
EXTRACTION←STABILISED WET SKIN
I DRY ↓
DRY SKIN

SOLVENT EXTRACTION

∟► DESOLVENTISATION
(REDUCED PRESSURE)
COLORANT
The novelty of the present invention is that the chlorophyll present in hitherto unexplored edible plant source, namely fresh green pepper skin is stabilised and subsequently processed to get a green colorant for food use.
The invention is illustrated by the following examples which should not, however, be construed to limit the scope of the present invention.Processing conditions with reference to two examples are given below.
Example 1
One kg of fresh pepper spikes were destalked manually and cleaned using running cold water to get 770 gm cleaned berries. The berries were immersed in 2 liters of water in a steam jacketed kettle and temperature was raised to 98°c and held for 20 minutes. The blanched berries were then washed with running cold water and passed through a pulper to obtain 400 gm of pulp which was treated with 400 ml of 1% solution of potassium meta bisulphite in water and held for 4 hours at a pH of 3.5. The pH of the separated [pulp was raised to 10 by the addition of sodium carbonate solution, held for 20 minutes, washed and pressed to retrieve the colour stabilised wet pulp(160g) Colour stabilised wet pulp (80g) was extracted with 240 ml of acetone and desolventised to get 2.5 gm colorant in paste form. The other part of the colour stabilised pressed wet pulp (80g ) was dried at 45°C for 4 hours to obtain a dry powder (40g) which was extracted with 200 ml of aqueous acetone and desolventised to get 2.5 gm colorant as a resinous mass.
Example 2
Five hundred gram of fresh pepper spikes were destalked manually and cleaned using running cold water to get 400 gm of berries. The berries were subjected to a temperature of 170°c for 3 minutes cooled to room temperature
and passed through a pulper to get 160 gm pulp which was treated with 160 ml of 0.5% solution of potassium meta bisulphite and held for 4hours at a pH of 4.0 . Separated pulp was treated with sodium carbonate solution to pH of 10 for 30 minutes and washed and pressed and dried at 50° C for 4 hours to retrieve 40 g pulp. The dry pulp was extracted with 200 ml of aqueous alcohol and desolventised to get 2.5 gm colorant as a resinous mass. The main advantages of the present process invention are
(a) It is possible to get a natural green colorant for food use from an edible
plant material which was not explored so far for this purpose.
(b) The chlorophyll in the plant material is stabilised, pungent constituents
co-occuring with the pigment are removed and the bland stabilised skin
is used for colour extraction, either as such or after drying .
(c) The green skin obtained as a waste product from the process
of making white pepper is suitably processed for colour extraction.



We claim:
1. A process for the preparation of stable natural green colorant from the skin of fresh green pepper berries which comprises the steps of:
(a) bleaching of fresh green pepper berries in water at a temperature in the range of
90-100 deg C for a period of 10-30 minutes or heating of fresh green berries at
a temperature in the range of 140 - 210 deg C for a period of 10-20 minutes,
(b) removing the skin from the bleached berries obtained in above step (a) in a
known method mechanically or manually to obtain wet mass of skin,
(c) stabilizing the above said wet mass of skin using stabilizing agent such as
sulphur dioxide selected from potassium meta bisulphite and sodium meta
bisulphite at the concentration in the range of 0.01-1 percent at a pH of 3-6
(d) alkalizing said stabilized wet mass of skin obtained in above step (c) with an
aqueous solution of meta salts selected from carbonate and bicarbonate of
sodium and potassium at a pH of 7.5 - 11.0
(e) drying the wet mass of skin obtained in step (d) to obtain dried mass of skin
using a mechanical drier in known method at the temperature in the range of
40-60 deg C for a period of 6-8 hours,
(f) extracting the colorant from the dried mass of skin obtained in step (e)using
solvent selected from non-polar group consisting of hexane, ethyl ether,
petroleum ether and polar solvent selected from group consisting of methyl
alcohol, acetone and water; and
(g) removing the solvent at low temperature in the range of 20-27 inches of mercury to get desired resinous mass rich in green colourant having chlorophyll content of 1-1.7%.
2. A process as claimed in claim 1, the yield of the colourant is in the order of
0.5% fresh green berries.
3. A process as claimed in claims 1&2, wherein bitching of fresh green berries is
preferably carried out at 96-98 deg C for a period of 10-15 minutes.
4. A process as claimed in claims 1-3, wherein concentrate of chemical stabilizer
used is preferably in the range of 0.05-0.07%
5. A process as claimed in claims 1-4, wherein alkalization is carried out at pH
preferably in the range of 7.5-9.0
6. A process as claimed in claims 1-5, wherein the resinous green colour obtained is
rendered more useful for food application using a medium of edible oil, fat, fatty
acid and permitted emulsifiers for imparting a green or yellowish green colour to
selected foods.
7. A process for the preparation of stable natural green colourant from the skin of
fresh green pepper berries substantially as herein described with reference to the
accompanying examples.

Documents:

386-del-2001-abstract.pdf

386-del-2001-claims.pdf

386-del-2001-correspondence-others.pdf

386-del-2001-correspondence-po.pdf

386-del-2001-description (complete).pdf

386-del-2001-form-1.pdf

386-del-2001-form-18.pdf

386-del-2001-form-2.pdf

386-del-2001-form-3.pdf

386-del-2001-petition-137.pdf

386-del-2001-petition-138.pdf


Patent Number 231591
Indian Patent Application Number 386/DEL/2001
PG Journal Number 13/2009
Publication Date 27-Mar-2009
Grant Date 06-Mar-2009
Date of Filing 29-Mar-2001
Name of Patentee COUNCIL OF SCIENTIFIC AND INDUSTRIAL RESEARCH
Applicant Address RAFI MARG, NEW DELHI-110001, INDIA.
Inventors:
# Inventor's Name Inventor's Address
1 SATHYAGALAM RANGANATHA DESIKACHARYA SAMPATHU CENTRAL FOOD TECHNOLOGICAL RESEARCH INSTITUTE, MYSORE
2 SRINIVASAN LAKSHMI NARAYANAN CENTRAL FOOD TECHNOLOGICAL RESEARCH INSTITUTE, MYSORE
3 HALAGUR BOGEGOWDA SOWBHAGYA CENTRAL FOOD TECHNOLOGICAL RESEARCH INSTITUTE, MYSORE
4 NANJUNDAIAH KRISHNAMURTHY CENTRAL FOOD TECHNOLOGICAL RESEARCH INSTITUTE, MYSORE
PCT International Classification Number C09B 61/00
PCT International Application Number N/A
PCT International Filing date
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 NA