Title of Invention

AN IMPROVED PROCESS FOR THE PRODUCTION OF BETALAINS DYE

Abstract The present invention provides to an economic process for the preparation of stable dry powder of betalains dye from red beet roots by avoiding the use of organic solvents, water or acidulated water. It is obtained by mixing juice of beet roots, directly with 1% to 2.5% of novel adsorbent such as gum acacia and soluble starch.
Full Text The present invention relates to an improved process for the production of betalains dye.
The present invention particularly relates to an economic process for the preparation of stable dry powder of betalains dye from red beet roots by avoiding the use of organic solvents, water or acidulated water. It is obtained by mixing juice of beet roots, directly with 1% to 2.5% of novel adsorbent $ucn as1 gum acacia and soluble starch.
Most varieties of beet root contain Betalains, which comprise of red betacyanins, betanins and the yellow betaxanthins i.e. vulgaxanthin I & II. Red betacyanin & betanins represent 75-90% of total colour present in beet root.
Beetroot is an excellent source of colour and some varieties contain colouring material upto 200 mg/100 gm. of fresh weight of beet root.
In India most of the red beetroot produced is used as vegetable and also in salads.
Beet root dye is used as powder in dairy and frozen products, It is also used in colouring hard candies, fruit chews, yoghurt, ice creams and salad dressings. Since betalains are highly colour intensive, these are used in very low doses, ranging from 5 to 20 ppm, as compared to some of the synthetic colouring dyes, which require high dose of colour, ranging from 20 to 100 ppm for the same colour intensity.(Hendry, G.A. F. & Houghton, J.D. (Ed.) Natural Food Colorants IInd. ed. Blackie Academic & Professional, London (1996) 61)
Beetroot juice as a spray dried powder is usually offered for sale, with specifications showing total betalain content. This dried power of beet root juice is prepared by adding malto-dextrine as an agent to absorb water. The quantity of malto-dextrine added is greater than the quanity of water removed during drying. .(Hendry, G.A. F. & Houghton, J.D. (Ed.) Natural Food Colorants End. ed. Blackie Academic & Professional, London (1996) 61)
In literature beet roots are processed for juice production using either mechanical expression or diffusion techniques. The juice is then centrifuged, pasteurized and concentrated, yielding approximately 70% sugar and 0.5% -1% betalains.

Purification of betalains for separation of betacyanin and betaxanthin is not necessary, when the dye is used commercially, however their separation is matter of interest for qualitative and quantitative analysis. Preliminary separation of betalains in beetroot juice has been accomplished by non-ion absorption on strongly acidic resins (Dowax 50w) followed by polyamide column chromatography. { Piattelli, M. and Minale, L. Phytochem. 3(1964) 307-311,547-557.}
Adams and Von-Elbe{ Adams, J. P. & Von Elbe, J.H., J. Food Sci. 42 ,NO 2 (1977), 410-14} reported that Gel filtration column chromatography on sephadex or polyacrylamide (bio-Gel P-6) gels could be used to separate betalains from beetroot juice.
Numerous other chromatographic and electro-phoretic procedures have been used to separate and purify the betalains from variety of sources. Now -a -days HPLC technique is being broadly used, as an efficient and rapid tool for the separation and analysis of betalains.
In 1975 oszlanyi et al {Oszlanyi, E., Karovic, V. (Czech) 155, 911 (Cl .A 231) 15 Nov. 1974; App. 23417 71 1st April 1971} have soaked beetroot juice with starch and the paste was dried under low temperature. The starch stabilizes the pigment. In 1987, Segal et al {Segal, B., Segal, R., Dima, G., Bentz, C., Voicila, I. & Robescu, C. (Interprindereade Prelucraresi Industrilizare a Legumelorsi Fructelor, Rimnicusarat) Rom. RO. 86,817(C1. C09B 61a700) 17th April 1985; App. 109370, 20th Dec. 1982} gave method for dye concentrate from beet roots by using fermentation technique.
In 1994 Kochneva et al {Kochneva, S. V.,D Ykaonova, V.K. (USSR) Razrab,K., Produktov, P. Dokl. 4 Vses Nauch - Tekhn.Konf, Razd. Zb. Kemerovo (1991), 66-8 (Russ.)} gave method for spray drying of natural food colourants, after converting its sugar to alcohol by fermentation.
In 1995 Czapski et al {Czapski, J., Sobkowska, E., Formanowicz, M. (Akademia Rolnicza) Pol. PL. 160304 (Cl. C09B 61/00)} have given method for isolating red dyes from beetroots by precipitating with organic solvents.
In 1996 Nita Marin et al {Nita Marin, G., Stefan, D., Cozma, D., (InterprindereaPlafor. Brasov) Rom. RO. 105,007 (C1A23LI/27) 1st Nov. 1994 ., App. 139,002 30th March 1989} have extracted dye with acidulated

water (pH 2-2.5) at 90°C followed by filtrate sedimentation, centrifuging and concentration of supernant in vacuum. In 1996 Czapski et al {Czapski, J., Sobkowska, E. (Akademia Rolnicza Pol.) Pol. PL. 167, 525 (Cl.C 12P1/00) 30th Sep. 1995,App. 292,732,10th Dec. 1991} obtained dye after juice was acidified, pasteurized and fermented under anaerobic conditions using wine yeast.
The juice can be spray-dried to a powder although malto-dextrine has to be added as a carrier since the high sucrose content precludes direct drying of the juice.
The amount of malto-dexrtine required is greater than the quantity of water removed during drying. { Hendry, G.A. F. & Houghton, J.D. (Ed.) Natural Food Colorants End. ed. Blackie Academic & Professional, London (1996) 61}
Beet root juice with only malto-dextrine as carrier/ water absorbing agent, is known in literature and as stated above with reference, the amount of this carrier used is very high and greater than the quantity of water removed from the juice during drying. While as in the present invention, authors have used novel adsorbents such as gum acacia and soluble starch in very low percentages (1% to 2.5 %) to adsorb the dye.
However following disadvantages have been observed in the processes described in the prior art.
1 .Generally water or acidulated water at 90° C is being used during expulsion of juice from beet roots, resulting in deterioration of the quality of the product and making it energy intensive during concentration.{ NitaMarin, G., Stefan, D., Cozma, D., (Interprinderea Plafor. Brasov) Rom. RO. 105,007 (C1A23LI/27) 1st Nov. 1994 .,App. 139,002 30th March 1989.}
2.Some methods of extraction have used organic solvents, which leave residual effect of solvent making them harmful for edible purposes. {Czapski, J., Sobkowska, E., Formanowicz, M. (Akademia Rolnicza)Pol. PL. 160304 (Cl. C09B 61/00)}

3.Recovery of betalains by existing mechanical /hydraulic pressing is not more than 50%. { Hendry, G.A. F. & Houghton, J.D. (Ed.) Natural Food Colorants Ilnd. ed.Blackie Academic & Professional, London (1996), 290}
4.In fermentation process for dye recovery, ethanol is produced as byproduct, which is difficult to remove from the dye. { Segal, B., Segal, R., Dima, G., Bentz, C., Voicila, I. & Robescu, C. (Interprindereade Prelucraresi Industrilizare a Legumelorsi Fructelor, Rimnicusarat) Rom. RO. 86,817(C1. C09B 61a/00) 17th April 1985; App. 109370, 20th Dec. 1982}
5.During spray drying Malto-dextrine has been used in high concentrations to the tune of water content present in the juice {Hendry, G.A. F. & Houghton, J.D. (Ed.) Natural Food Colorants End. ed.Blackie Academic & Professional, London (1996) 61} making product very costly,which has been avoided in the present invention.
6.Storage of spray dried dye has been carried at -23° C under Nitrogen atmosphere, which makes dye storage more difficult. {Singer, J. W., von ELBE, J.H., J.Food Sci. Vol. 45 ,489-491, Degradation rates of Vulgaxanthine 1}
The novelty of this invention resides in the use of adsorbing agent having melting point more than 160°C preferably gum acacia or soluble starch, adsorbing the dye.
The main objective of the present invention is to provide a process for the production of dry powdered betalains dye from red beet root by spray drying method without the use of organic solvents, water or acidulated water.
The another objective is to use novel adsorbents such as gum acacia and soluble starch in very low percentages (i.e. 1% to 2.5%) and spray drying the material into a uniform dye powder.
Yet another objective is to get powder having uniform hue and is stable at ambient temperature.
Still another objective is to make the process cost effective.

Accordingly the process for the production of dry betalains dye described in the present invention comprises of the following steps:
1. Blanching, slicing and mechanical pulping of red beet roots.
2. Expulsion of raw red beet root juice with novel adsorbents such as gum acacia or
soluble starch in very low percentages, (i.e. 1% to 2.5%) not used herein before.
3. Mixing of raw red beet root juice with novel adsorbents such as gum acacia or
soluble starch in very low percentages, (i.e. 1% to 2.5%) not used herein before.
4. Spray drying of the said adsorbent mixed juice in the spray dryer.
Accordingly the present invention provides an improved process for the
production of betalains dye, which comprises of blanching the beet roots using boiling water for a period of 2 minutes, expelling the juice from said blanched beet roots by conventional manner such as herein described, mixing the obtained juice with novel adsorbent selected from gum acacia, soluble starch having melting point above 160°C, in the range of 5 grams to 12.5grams/500ml, followed by spray drying at a temperature ranging 160°C - 170°C to get betalain dye.
In an embodiment of the present invention, the blanching may be carried out by exposing the beet roots in boiling water for two minutes.
In another embodiment, expelling the juice from blanched beet roots may be effected by crushing and centrifuging the pulp.
In yet another embodiment spray drying may be carried out in a spray dryer at chamber temperature of 160°C - 170°C.
The process of the preparation of dry powder of betalains dye from beet root juice is described in detail as given below which is provided by the way of examples for illustrations only and therefore should not be construed to limit the scope of the present invention.

JUICE EXTRACTION
Beet roots were thoroughly washed with water and then blanched (boiling for 2 min. in water). The blanched beet roots were sliced and subjected to mechanical pulping. The pulp along with juice was centrifuged to get clear juice. The recovery of juice was around 55-60% of the fresh weight of beet root. The juice was subjected to spray drying using various adsorbents in varying percentages. The objective of spray drying was:
1 .To get the betalains dye in powder form.
2.To find the optimum ratio of adsorbent and the juice.
3. To find out quantity and quality of betalains dye obtained by using various percentage concentration of adsorbent.
SPRAY DRYING
EXPERIMENT -1
500 ml of freshly expelled beet root juice obtained from 900 grams of red beet root was mixed with 12.5 grams (2.5%) of gum acacia. The contents were homogenized in a mixer and the homogenous solution was pumped into the spray dryer at a flow rate of 1 Lit/Hr. The chamber temperature of spray drier was maintained at 160° C with outlet temperature of 70°C. Time taken for the operation was around 30 minutes.The total spray dried material was 15 grams and its OD at 537nm was 0.402 and the percentage of betalains content was 0.718.
EXPERIMENT - 2
500 ml of freshly expelled juice was mixed with 5 grams (1%) of gum acacia. The contents were homogenized in a mixer and the homogenous solution was pumped into the spray drier at a flow rate of 1 lit/ Hr. The chamber temperature of spray drier was maintained at 160° C with outlet temperature of 70°C. Time taken for the operation was around 30 minutes. The total spray dried material obtained was 21 grams and its OD at 537nm was 0.412 and betalains content was 0.736%.

EXPERIMENT -3
500 ml of freshly expelled beet root juice was mixed with 12.5 grams (2.5%) of Soluble starch. The contents were homogenized in a mixer and the homogenous solution was pumped into the spray drier at a flow rate of 1 lit/ Hr. The chamber temperature of spray drier was maintained at 160° C with outlet temperature of 70°C. Time taken for the operation was around 30 minutes.The total spray dried material obtained was 12 grams and its OD at 537nm was 0.4o6 and betalains content was 0.728%.
EXPERIMENT -4
500 ml of freshly expelled beet root juice was mixed with 5 grams (1%) of soluble starch. The contents were homogenized in a mixer and the homogenous solution was pumped into the spray drier at a flow rate of 1 lit/ Hr.The chamber temperature of spray drier was maintained at 160° C with outlet temperature of 70°C. Time taken for the operation was around 30 minutes.The total spray dried material obtained was 18 grams and its OD at 537nm was 0.416 and betalains content was 0.743%.
EXPERIMENTAL RESULTS IN TABULAR FORM.
Amount Name %of Quantity Colour % Betalains
of juice of carrier of dried intensity
Expt. carrier material ODat
No. 537nm
1. 500ml Gum 2.5% 15 grams 0.402 0.718
Acacia
2. 500ml Gum 01% 21 grams 0.412 0.736
Acacia
3. 500ml Soluble 2.5% 12 grams 0.406 0.728
Starch
4. 500ml Soluble 01% 18 grams 0.416 0.743
Strach

ADVANTAGES OF OUR PROCESS
1 .No water, acidulated water or hot conditions have been used during extraction which makes the process energy effective and quality of the dye does not get impaired.
2.No organic solvents have been used for the extraction of juice making the product safe for edible purposes.
3.Juice recovery by mechanical pulping followed by centrifuging is 55-60% of fresh beetroot by weight.
4.Keeping in view the cost of the adsorbents, it was found that Gum-acacia is the best and the cheapest carrier for getting quality product at low cost.
5.Betalains dye obtained contains 0.4% to 0.8% pure betalains and the dye powder is quite stable at ambient temperature.



We Claims:
1. An improved process for the production of betalains dye, which comprises
of blanching the beet roots using boiling water for a period of 2 minutes,
expelling the juice from said blanched beet roots by conventional manner
such as herein described, mixing the obtained juice with novel adsorbent
selected from gum acacia, soluble starch having melting point above
160°C, in the range of 5 grams to 12.5grams/500ml, followed by spray
drying at a temperature ranging 160°C - 170°C to get betalain dye.
2. An improved process as claimed in claim 1, wherein conventional method
used for expelling the juice from blanched beet roots is crushing and
centrifuging the pulp.
3. An improved process as claimed in claims 1-2, of the present invention,
spray drying is carried out in a spray dryer.
4. An improved process for the production of betalains dye from red beet
roots, substantially as herein described with reference to the examples
accompanying this specification.


Documents:

661-del-2000-abstract.pdf

661-del-2000-claims.pdf

661-del-2000-correspondence-others.pdf

661-del-2000-correspondence-po.pdf

661-del-2000-description (complete).pdf

661-del-2000-form-1.pdf

661-del-2000-form-19.pdf

661-del-2000-form-2.pdf

661-del-2000-form-3.pdf


Patent Number 217127
Indian Patent Application Number 661/DEL/2000
PG Journal Number 13/2008
Publication Date 31-Mar-2008
Grant Date 25-Mar-2008
Date of Filing 18-Jul-2000
Name of Patentee COUNCIL OF SCIENTIFIC AND INDUSTRIAL RESEARCH
Applicant Address RAFI MARG,NEW DELHI-110 001, INDIA
Inventors:
# Inventor's Name Inventor's Address
1 VIRANDER KUMAR KOUL REGIONAL RESEARCH LABORATORY, CAURL ROAD, JAMMU - 180000
2 MAHABIR PRASAD JAIN REGIONAL RESEARCH LABORATORY, CAURL ROAD, JAMMU - 180000
3 SUMAN KAUL REGIONAL RESEARCH LABORATORY, CAURL ROAD, JAMMU - 180000
4 VIJAY KUMAR SHARMA REGIONAL RESEARCH LABORATORY, CAURL ROAD, JAMMU - 180000
5 CHUNNI LAL TIKOO REGIONAL RESEARCH LABORATORY, CAURL ROAD, JAMMU - 180000`
6 SATINDER MOHAN JAIN REGIONAL RESEARCH LABORATORY, CAURL ROAD, JAMMU - 180000
7 SURESH CHANDRA REGIONAL RESEARCH LABORATORY, CAURL ROAD, JAMMU - 180000
PCT International Classification Number A23L 1/00
PCT International Application Number N/A
PCT International Filing date
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 NA