organic lycopene patent usa

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The Director of the United States Patent and Trademark Office Has received an application for a patent for a new and useful invention. The title and description of the invention are enclosed. The requirements of law have been com- plied with, and it has been determined that a patent on the invention shall be granted under the law. Therefore, this U nited States Patent Grants to the person(s) having title to this patent the right to exclude others from mak- ing, using, offering for sale, or selling the invention throughout the United States of . America or importing the invention into the United States of America, and if the inven- tion is a process, of the right to exclude oth- ers from using, offering for sale or selling throughout the United States of America, or importing into the United States of America, products made by that process, for the term setforth in 35 Us.c. 154(a)(2) or (c)(1), subject to the payment of mainte- nance fees as provided by 35 Us.c. 41 (b). See the Maintenance Fee Notice on the inside of the cover. Director ofthe Uni/ed Sta/es Paten/ and Trademark Ojjìce

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The Director of the United StatesPatent and Trademark Office

Has received an application for a patent fora new and useful invention. The title anddescription of the invention are enclosed.The requirements of law have been com-plied with, and it has been determined thata patent on the invention shall be grantedunder the law.

Therefore, this

United States Patent

Grants to the person(s) having title to thispatent the right to exclude others from mak-ing, using, offering for sale, or selling theinvention throughout the United States of

. America or importing the invention into theUnited States of America, and if the inven-tion is a process, of the right to exclude oth-ers from using, offering for sale or sellingthroughout the United States of America, orimporting into the United States ofAmerica, products made by that process,for the term setforth in 35 Us.c. 154(a)(2)or (c)(1), subject to the payment of mainte-nance fees as provided by 35 Us.c. 41 (b).See the Maintenance Fee Notice on theinside of the cover.

Director ofthe Uni/ed Sta/es Paten/ and Trademark Ojjìce

MAINTENANCE FEE NOTICEIf the application lor this patent was filed on or after December 12, 1980, maintenancelees are due three years and six months, seven years and six months, and eleven years andsix months after the date 01this grant, or within a grace period 01six months thereafterupon payment oj a surcharge as provided by law. The amount, number and timing 01themaintenance lees required may be changed by law or regulation. Unless payment oj theapplicable maintenance lee is received in the United States Patent and Trademark Officeon or belore the date the lee is due or within a grace period oj six months thereafter, thepatent will expire as 01the end 01such grace period.

PATENT TERM NOTICEIf the application jor this patent was filed on or after June 8, 1995, the term oj thispatent begins on the date on which this patent issues and ends twenty years from thefiling date 01 the application or, if the application contains a specific rejerence to anearlier filed application or applications under 35 USc. 120, 121, or 365(c), twentyyears jrom the filing date 01 the earliest such application ("the twenty-year term "),subject to thepayment ojmaintenancelees as provided by 35 Us.c. 41 (b), and anyextension as provided by 35 US.c. 154(b) or 156 or any disclaimer under 35 USc.253.

If this application was filed prior to June 8, 1995, the term oj this patent begins on thedate on which this patent issues and ends on the later oj seventeen years from the date01the grant oj this patent or the twenty-year term set jorth above jor patents resulting!rom applications filed on or after June 8, 1995, subject to the payment oj maintenancelees as provided by 35 US C. 41 (b) and any extension as provided by 35 US C. 156 orany disclaimer under 35 Us.c. 253.

(12) United States PatentRescio

111111111111111111111111111111111111111111111111111111111111111111111111111US008263156B2

(10) Patent No.:(45) Date or Patent:

US 8,263,156 B2Sep.ll,2012

(54) FOOD SUPPLEMENT BASED ONBIOLOQICALLYCOPENE AND PROCESS TOOBTAIN BIOLOGICAL LYCOPENE

(76) Inventor: Leonardo Rescio, Corigliano d'Otranto(lT) .

/

( *) Notice: Subject to any disclaimer, the term of thispatent is extended or adjusted under 35U.S.C. 154(b) by 726 days.

(21) Appl. No.: 12/309,905

(22) PCT Filed: Oet. 20,2006

(86) PCT No.: PCTIIB2006/003390

§ 371 (c)(1),(2), (4) Date: Feb. 2, 2009

(87) PCT Pub. No.: W02008/015490

PCT Pub. Date: Feb. 7, 2008

(65) Prior Publieation Data

US 200910304870 Al Dec. lO, 2009

(30) Foreign Applieation Priority Data

Aug. 2, 2006 (IT) :. BA2006AOO49

(51) Int. Cl.CllB 1110 (2006.01)A23L 1/222 (2006.01)

(52) V.S. Cl. 426/489; 426/615; 426/429; 426/478;426/495

(58) Field of Classifieation Seareh 426/648,426/615,425,429,478,489,492

See applieation file for complete search history.

(56) Referenees Cited

U.S. PATENT DOCUMENTS5,897,866 A'" 4/1999 Bombardelli et al 424/7776,515,018 BI'" 2/2003 Fuhrman et al. 514/458

_b:co,

.I

7,672,468 B2 * 3/2010 Kaiser et al 381/3142003/0180435 Al * 9/2003 Shi 426/6152005/0266132 Al * 12/2005 Temelli et al 426/4782009/0297683 Al'" 12/2009 Zelkha et al 426/580

FOREIGN PATENT DOCUMENTSWO W001/79355 * 10/2001

OTHER PUBLICATIONS

Vasapollo, G. et al. 2004. Journal of Supercritical Fluids 29:87.*Anon. 1982. The Arnerican Heritage Dictionary, 2nd edition,Houghton Miffiin Co., Boston. p. 1061.*

.•.cited by examiner

Primary Examiner - Carolyn Paden(74) Attomey, Agent, or Firm - R.Ruschena Patent Agent,LLC

(57) ABSTRACT

Innovative food supplement based on biological lycopene,which is the bulk product, i.e. the total extract, obtained bytreating with supercritical carbon dioxide a suitable extrac-tion matrix, made by 50% biological tornato berries and 50%biological dry fruits (almonds, nuts and the like) and/or othercomponents, following a co-extractive technology. Tornatoberries are conveniently de-hydrated, milled and riddled; theco-extraction matrix (dry fruits, vegetables; others) is conve-niently de-hydrated and milled. The obtained total extract isdirectly used for preparing lycopene based food supplements,without any modification or additivation. With respect to theknown commerciai food supplement, based on lycopene,such biologicallycopene has unique quality features: the totalextract is 100% natural; absence of chemical solvents; lyco-pene concentration in the final natural formula (not artificial);absence dosing problerns and contra-indications. In the finalproduct, lycopene is mixed with other natural anti-oxidants,co-extracted from the used vegetables. The boxing up ofthebulkproduct (total extract) is made in soft or-hard caps inseveral shapes and colors or in tablets or in other way (e.g.liquid, others).

5 Claims, 1 Drawing Sheet

co, lUoycle

Irrapurity(Weter,eutraiDers,cosolvcuts"etc.)

FracDon 1 Fraction2

v.s. Patent Sep.ll,2012 US 8,263,156 B2

US 8,263,156 B21

FOOD SUPPLEMENT BASED ONBIOLOGICALLYCOPENE AND PROCESS TO

OBTAIN BIOLOGICAL LYCOPENE

BACKGROUND OF THE INVENTION

Technical Field

The present invention relates to a new food supplement,based on biological lycopene.

In the state ofthe technique, antioxidants, that reduce oxi-dative damage to ceIIs are qui te k.nown. They are both naturalor synthetic products. WeII-k.nown natural antioxidants arethe Ascorbic acid (C-vitarnin), Tocopherol (E-vitarnin), Ret-inol (A-vitarnin) and Beta-Carotene. One major action of 15antioxidants is to prevent damage due to the action of Oxygenfree radicals, which can damage celIs by chernical chainreactions. In addition, antioxidants play an important role inpreventing celI aging, arteriosclerosis, cancer and heart dis-eases. Antioxidant can be found in many vegetables and 20fruits, among which, tomatoes synthesise a large antioxidantquaIity. Tornato, in fact, is considered a healthy food due tothe fact that it (and its derivatives: peel tomatoes, tomato-sauce, tomato-juice, and simiIar) are rich sources of caro-tenoids. Carotenoids are composed of a rnixture of Carbon, 25Hydrogen and sometimes Oxygen. These molecules are builtby vegetables, by utilizing simpler molecules; they areresponsible for the colours of ftowers, fruits, and some roots.For exarnple, carrots gain their orange colour from beta-carotene, the first carotenoid to be isolated at the pure state, 30wruch gives the name to the carotenoid farnily. One of thecarotenoids, characterized by high antioxidant property islycopene, which provi de the pigrnent of the red colour. Fruitsand vegetables that are high in lycopene include strawberry,papaya, water-melon, grapefruit and similar. Among which, 35red tomatoes have the highest concentration of lycopene(from 30 to 400 mg/kg of fresh tornato), which is easiIyassirnilated by the human body in high percentage whenfresh, and a!most totally upon cooking andlor served in oiI-rich dishes for fatty acids generally increases assirnilation. 40Clinica! studies have proved that highly benefici al effects oflycopene to prevent some kinds of cancer and other cardio-vascular diseases; and to slow down natural celI aging pro-cesso Lycopene, in fact, plays an important protective role forhis high and specific antioxidant property.

It is a!so known that lycopene is employed as a basic rawmaterial to prepare food supplements, by means of chernicalsynthesis (synthetic lycopene) or vegetable bio-synthesis(natura! lycopene). In the latter case, the extraction of naturallycopene from vegetables (e.g., tornato) ismade by using 50chernical solvents.

Synthetic lycopene is obtamed by means of chernica! reac-tions, known in literature as "Witting process". It is a quitelong and complex process, wruch comprises the production oftwo intermediates, which react with a third compound yield- 55ing raw lycopene, which is, finaJly, purified by filtration andrecrystallization. The end product is a red crystalline soli d,characterized by large needle-shaped regular and clean crys-tals, and a final lycopene concentration of about 95% (impu-riti es and chernical solvents==5%). Lycopenes are marketed as 60food colorants (sauces, ketchup, enriched in lycopene) and asan ingredient in food supplement.

The production process of "natura!" lycopene starts fromfresh tornato (which can be OGM or treated with pesticidesand other phytomedicines), which is rninced, homogenized 65and the centrifuged to remove most of the water. The residua!hurnid pasta is the tornato concentrate. Lycopene extraction

2from the tornato concentrate is made by adding organic sol-vents with strong agitation. Obviously, together with the lyco-pene, other lipidic substances and the soluble phytomedi-cines, are extracted as welI. Afterwards, by adding water, the

5 solution is separated in two phases: an organic one, consisting·of a solution of organic solvents with lycopene and the othersubstances extracted, and a Iiquid phase containing water and(he insoluble vegetable residua!. By reducing the solubiIity bysolvent evaporation or other, an amorphous precipitate is

lO obtained from the lycopene organic phase; such precipitate(as for the synthetic lycopene) can be purified and recrystal-lized. The end product has a red-brown colour, partially crys-talline, containing chernical solvents and characterized bydirty crystals (impurity inclusions and solvents), more or lesslarge and regular and with a lycopene concentration of about60%.

The above described lycopene extraction processes presentsevera! drawbacks, in terms of efficiency and above ali qualityof the final product.

Generally, the purity of crystal-shaped end product mainlydepends on the purity of the raw materials used and thecrystallization and purifying processes adopted. If necessaryor convenient, the recrystallization of the end product can berepeated. In the synthesis process, the used raw materials area!most pure; therefore, even with more steps, it is easy toobtain a crystalline solid with 95% purity. On the other side,given the high toxicity of the raw materials (aldehydes andsirnilar) and the solvents used (e.g., toluene) the end productneed to be further purified to reduce its toxicity. Moreover, ifthe synthetic lycopene in crystal is improperly stored (ex-posed to Iight or air), it can degrade in mutagenic products;therefore, it is necessary to add antioxidants to prevent orreduce this effect.

In the case of lycopene obtained by the natural process, itstoxicity is due both to the chernical solvent residuals in theend product and to the used raw material quality. In fact,tornato berries could have been treated with pesticides andother phytomedicines, would be extracted together with Iyco-pene and be concentrated in the end product. In trus process,the lycopene extraction from the tornato berries is made withone or more organic solvents; since in the biological matrix,together with lycopene, there is a large quantity of solublelipidic substances, which are extracted together with the lyco-pene. Impurities are natural and not toxic, but, proportionalIy

45 to their quantity, large quantity of toxic and harmful chernicalsolvents are also adsorbed. Moreover, oxidation productscould be yielded during the process which are very toxic. Thenatural Iycopene, obtained by re-crystaliization, could bepurified, with an efficiency loss (10-20 in percentage, for eachstep).

SUMMARY OF THE INVENTION

The present invention aims at creating a new product, to beemployed as food supplement, based on "biological" lyco-pene; and of related natural extraction process of lycopene,which can assure very high purity and quality together with asatisfactory extraction efficiency.

The present invention sol ves the problems, related to lyco-pene extraction, being a food supplement, based on biologicallycopene, which is extracted t'rom a suitable extraction mate-rial (totally or partialIy vegetable) by means of supercriticalcarbon dioxide and co-extraction technology. The extractionmaterial to be treated. with supercritical carbon dioxide, ismade of a mixture, said mixture composed of an extractionmatrix and a co-extraction matrix, in the same or differentquantities.

3US 8,263,156 B2

4Moreover, another object of the invention is the extraction

process of Iycopene, by means of carbon dioxide in super-criticaI conditions, from a suitable biological matrix. Thecarbon dioxide extrac~on from the above matrix leads to atotal extract with a Iycopene concentration ranging from 1 to 5

2%, according to the initial Iycopene concentration in thetornato berries. The end product is 100% natural and withoutany toxic or harmful chemical substance. For this reason, theIycopene is defined as 'biologica!'. The use of biologicalIycopene is particularly suitable as high quality food supple- IOment, as well as pharrnaceutical and cosmetic producI. Thequality of lycopene obtained by this process is so differentfrom the one obtained by the traditional processes, that this'biologica!' lycopene can be considered as a new producI.These and other advantages will be pointed out in the 15

detailed description of the invention, that will refer to tables1/4, 2/4, 3/4 and 4/4 in which some experimental results,arising from the process and the product, and an example ofthe apparatus realizing the co-extraction process are shown.Both are exemplifying and not restrictive.

BRIEF DESCRIPTION OF THE TABLES ANDDRAWINGS

With reference to the above mentioned tables:Tab1e l is a summary of the features of the synthetic,

natural and biological Iycopenes, used to prepare lycopenebased food supplements.

Table 2 shows some commerciai lycopene-based foodsupplements (US market, 2005). .

Table 3 is a biologicallycopene specification.Table 4 shows the carotenoid characterization.Table 5 shows the fatty acid characterization.FIG. 1 is the scheme of the apparatus realizing the extrac-

tion with supercritical ftuids.

DETAILED DESCRIPTION OF THE INVENTION

Thus, scope of the invention is a total extract from a suit-able extraction material, (totally or partially vegetable), by 40using supercritical carbon dioxide with the co-extractiontechnology. This extraction material is composed by the mix-ture of an extraction matrix and a co-extraction matrix, eachof them in the same or in different amounts. The extractionmatrix is made of tornato berries, which are convenientlyprocessed (washed, purified, concentrated in chromoplàsts orother similar processes), dehydrated (cold or warrn process,in air or in vacuum, by evaporation, sublimation or othersimilar process), milled and riddled. The co-extraction matrixcan be totally made of each of the following materials or anypossible combination between them:

dry fruit, made of single seeds of peanuts, nuts, almonds,walnuts, pistachios and sirnilar, or any mixing betweenthem; .

oiIy seeds of sunflower, soy, water melon, citrus fruits,pumpkin, grapefruit, other oily seeds, or any rnixingbetween them;

leaves andlor branches andlor f10wers andlor roots andlorother parts of rosemary, sage, origan, garlic, carrots,cauliflower, other plants, taken alone or in any mixingbetween them;

fish meal.In ali cases, the material is conveniently processed, dehy-

drated and rnilled.A further scope of the invention is an optirnised process for 65

the lycopene co-extraction from tornato powder, by usingsupercritical carbon dioxide, consisting in the preparation of

the raw materials (first step) and the Iycopene extraction andseparation from the raw materials (second step), character-ised by the contemporary extraction of vegetable oil and otherdry fruit compounds andlor oily seeds andlor vegetables andsimilar. Operative conditions being equal, said vegetable oiIas co-solvent improves the lycopene extraction efficiency-up to 10% after 4 h extraction, up to 30% after 8 h extraction,up to 60% for a longer extraction duration-and preventsIycopene degradation. The extraction matrix is a rnixture oftornato powder and dry fruit andlor oily seeds andlor othervegetables andlor fish meal. The rnixture preparation com-prises raw material dehydration (vacuum dehydrated toma-toes, in cold or warm conditions, by evaporation, sublimationor other processes) and the'dry tomatoes milling and riddlingunti! a fine powder is obtained; rnixing of the obtained tornatopowder with the same quantity of dry fruit (almonds, nuts,peanuts and sirnilar) or oily seeds (sunflower seeds, and simi-lar) or vegetables or others and mixture milling. Said milltureis milled until a homogeneous pasta is obtained. The super-

20 critical carbon dioxide pressure ranges between 400 and 600bar; its temperature ranges between 320 and 373 K. Operativeconditions being equal, the carbon dioxide ftowrate rangesbetween 15 and 40 Kg CO2/h; and its density ranges between0.800 and 0.950 KgIl. The Iycopene extraction phases com-

25 prise: CO2 compression and heating, Iycopene and othercompounds extraction, mixture cooling, first separationphase, pressure reduction, second separation phase and col-lection of the solute, which precipitates from the mothersolution, further pressure reduction, third separation phase

30 with further collection of the solute, CO2 recycling and stor-age, after filtration and condensation.

The biological process is made with CO2, in a single stepand produces a total extract with a lycopene concentrationranging from 1 to 2%. The lycopene concentration in the end

35 oleoresin depends on the matrix properties used for theextraction (lycopene titre, berry quality and maturationdegree, pre-treating process). The end product is 100% natu-ral, without any chemical solvent or other toxic and harmfulimpuri ties.

The 1-2% lycopene concentration is well suitable for thedirect packaging of the product in soft caps or other specialty.

The extraction apparatus with supercritical f1uids, schema-tized in FIG. 1, comprises a lO l extractor (AOI) and threein-sequence separators (SI, S2), both 1.5 I, and (S3), 0.3 l,

45 respectively. Once the target pressure is reached by the pump(PI), the CO2 f10ws through a heating coil (E2) before reach-ing the extraction bed (AOI). Then, leaving (AOI), the f10wreaches the separator (SI), through a cooling coil (E3) and,then, the separator (S2), passing through a micrometer valve

50 (VL1), reducing CO2 pressure and density. Precipitating fromthe mother solution, the solute is collected in (S2). Then, theftuid f10w through the separator (S3), and the secondmicrometer valve (VL2), which reduces its pressure up to thefinal value; the separated solute is collected in (S3). Exiting

55 the separator (S3), CO2 can be recycled and collected in thetank (TOI), through the filter (FI) and the condenser (El).The separator (SI) works at a constant pressure; the tempera-ture variation reduces the extract solubility, causing its sepa-ration and precipitation. In the separators (S2, S3), the solu-

60 bility decreases by varying the pressure.The main difference between synthetic or natural Iyco-

pene, extracted by chernical solvents, and the biologicallyco-pene, obtained by supercritical CO2, is that in the first twoprocesses the purification phase is essenti al, while in thebiological process is useless and even damaging. In fact,differently from the other two processes, in the biologicalprocess alI the substances different from Iycopene are natural

5US 8,263,156 B2

compounds as well, which are important for individuaI bealthand well-being and empower the Iycopene anticancer activ-ity. They are phospholipids, Tocopherol (E-vitamin), omega 3and omega 6 poly-unsaturated fatty acids, other carotenoids(Lutein, Beta Carotene, and similar) extracted from veg- 5etables which pl~ an important role as antioxidants and aslipids, to enhance the lycopene absorption process throughthe tissues and, consequently, its transfer into the blood (bio-availability). The end product is 100% natural, without any

lOtoxicity and suitable to everybody.The pure or concentrated lycopene is not suitable for direct

use by humans, due to several reasons, among which the lowbio-availability. However, it is well known that Iycopeneabsorption by the tissues and its transfer into the blood is 15enhanced by lipidic substances (e.g., vegetable oil). In thepreparation of the synthetic Iycopene-based commerciaiproduct, the lipidic substances must be completely added, to

. dilute Iycopene crystals (almost pure) until the desired finalconcentration. In the case ofthe naturallycopene-based com-merciai product, the lipidic substances must be also added,even if partially already exisling in the product itself. On thecontrary, in the case of the biological Iycopene based com-merciai product, no addition of exogen lipidic substances isrequired, since the product contains the necessary lipidicsubstances. Lycopene structure is another important feature 25inftuencing the product bio-availability; in the Iycopene case,the structure can be crystalline, amorphous or mixed, withvariable crystal percentage. The crystalline structure is morestable than the amorphous one and requires more energy todissolve into molecules; and, for this reason, it shows less 30bio-availability than the amorphous structure, which is imme-diately available. The crystalline or amorphous structuresdepend on the Iycopene production process, the chemical-physical conditions and the management of the solute-solu-tion separation processo In the production process ofthe syn- 35thetic or natural Iycopene, its separation from the organicsolvent solution can vary in time, but the process always takestwo different steps: the nucleation and the crystalline growth.In these processes (synthetic and naturallycopene) the lyco-pene separation from the mother waters is made to get thepurest precipitate: all the substances beside Iycopene are 40toxic impurities and toxic and harrnful organi c chemical sol-vents. The end product is totally (synthetic Iycopene) or par-tially crystalline (naturallycopene). Instead, in the biologicalIycopene production process with supercritical carbon diox-ide, the lycopene separation from the solvent solution (C02) 45is instantaneous; in fact, the Iycopene solubility in the CO2

solution depends on the density (0,8-0,95 kgll), whichdepends on the pressure (400-600 bar) and the temperature(320-373 K); in the separator, pressure is rapidly reduced upto 70-150 bar, causing the density reduction up to O, l kgll or 50less, and this causes the immediate precipitation of the solutes(lipids and Iycopene), contained in the solution. Therefore,with this methodology, the standard solute-solution separa-tion process is no more needed, since the Iycopene immedi-ately precipitates in a 100% amorphous state. 55

Table l summarizes the lycopene characteristics accordingto the three production methodologies.

The Iycopene-based food supplements are obtained bydilution ofthe concentrated bulk Iycopene (synthetic ornatu-ral) with several additives or excipients up to the final con-centration value of the active principle (lycopene), which is 60desired in the formula. Nowadays, the marketed productsbased on synthetic or natural lycopene, contai n a Iycopeneweight pro dose ranging from l mg to IO mg, correspondingto a lycopene concentration in the end formula ranging fromless than 1% up to 10% (weight percentage). Table 2 shows 65that the US commerciaI products most required are Iycopenefood supplements in soft caps, rather than tabs or similar. On

6the contrary, the biologicallycopene-based food supplementrepresents a new product with respect to the known productson the market: il is exclusively composed of the total extract,which is obtained by treating with supercritical CO2 a suitablebiological matrix made of about 50% tornato berries, whichare conveniently dehydrated, milled and riddled, and about50% dry fruits (almonds, walnuts, nuts, peanuts, pistachioand similar) ancl/or oily seeds, ancl/or other vegetable or fishmeal, conveniently treated and milled. In particular, theextraction matrix is always composed of about 50% tornatopowder, while for the other part, it is possible to employ eitherjust one type of dry fruit or oily seeds or other vegetables orfish meal, or one of their possible mixture, so that in theextraction matrix the ratio tornato berries to the other is about1. .

Below some possible combinations are listed.l) Tornato powder and nuts2) Tornato powder and almonds3) Tornato powder and pistachio

20 4) Tornato powder and walnuts5) Tornato powder and peanuts6) Tornato powder and other oily seeds7) Tornato powder and dry fruit mixture and/or other oily

seeds8) Tornato powder and fish meal9) Tornato powder and fish meal and dry fruitslO) Tornato powder and vegetable oils and/or fish meal

A very important alternative of the extraction matrix is theaddition of fish meal to increase the percentage of poly-unsaturated fatty acids in the obtained extract. The Iycopene-concentration in the tornato powder can range from 5000 to15000 mg/kg. The obtained total extract represents the endproduct, which isdirectly packaged, without any modifica-tion of the composition by adding additi ves and similar. Thelycopene concentration in the total extract ranges from 1% to2%, depending on the Iycopene concentration in the treatedtornato berries. The carotenoids come entirely from thetornato. while the lipidic portion, the tocopherols (E vitamin),the poly-unsaturated fatty acids and other compounds comefrom both the tornato and the co-matrix.

Since the lycopene concentration in the final extractdepends on the Iycopene concentration in the fresh tornatoberries, in the extraction product the Iycopene concentrationis absolutely natural, as far the food supplements, synthetic ornaturallycopene based, where the Iycopene concentration inthe end formula can be easily varied, depending on theamount of additive (e.g., due to commerciai needs).

A further characteristic of the biological Iycopene, withrespect to the natural one, is the small time interval betweenthe C02 treatment of the matrix and the end product packag-ing.

The bulk biologicallycopene specification, which is alsothe specification of the final food supplement, is reported inTable 3. The quantity and the kind of carotenoids in the extractdepend on the variety of the tornato berry, its maturationdegree, the climatic and cultivation conditions and the pre-treatment. In Table 4 the share of the normally availablecarotenoids is shown. The quantity and the kind of the lipidicsubstances in the extract depend on both tornato berrilès char-acteristics and the.used co-matrix. In the case of a nuts co-matrix, the fatty acids composition is reported in Table 5. TheC02 extracted oleoresin. together with the carotenoids fam-ily, which is available in the fresh berry, also contains remark-able quantities of essenti al poly-unsaturated fatty acids(PUFA). They are: linoleic acid (omega-6) andalfa-linolenicacid (omega-3).

7US 8,263,156 B2

8TABLE l

Product Biological LycopeneSyntheti~ycopene Natura! Lycopene

Raw materia!

PtoductiontechnologyBulk end product

Bulk end productpurification

Commercia!formulaToxicity

Bio-availabilty

Natura!

Tornato berries (no.regulation).Use of OGM, pesticides,phytomedicines, etc., is possibleTornato e"traction with chemica!solvents (THF, etc.)Amorphous and crysta!line.Irregular and dirty crystals.. Lycopene: 50-60%. Impurities andchemical solventsMandatory. Ali different fromIycopene are impurities and toxic-hannful chemical solvents1-10% Dilution, with lipids+other exogen chemical additivesPossible presence of impuritiesand toxic/hannful solvents(pesticides ?)Improved by exogen lipids andother chemical additives

Synthetic raw materials

Chemical synthesis reactionsbetween synthetic compoundsCrystalline. Clean, regular andbig crystals. Lycopene: 90-95%.Impurities and chemical solvents

Mandatory. Ali different fromIycopene are impurities and toxic-hannful chemical solvents1-10% Dilution, with lipids +other exogen chemical additivesPossible presence of impuritiesand toxic/hannful solvents

Improved by e"ogen lipids andother chemical additives

Zero. Completely syntheticproduct with possible impuritiesand chemical solvents

Certified biological tornatoberries. No OGM, pesticides,phytomedicines, etc.Biological tornato e.traclionwith supercritical C02Amorphous. Lycopenesuspension (1-2%) in tornatoNatura! Lipids

Not needed.100% natura! product

As extracted

Absent

Low. Natura! product withchemical solvents and exogenchemical additives

Optimal. Presence of Lutein,poly-unsaturated fat acids, E-vitamin, etc.Maximum. Only what is presentin the tomatoes is extracted,boxing up as it is

TABLE2

Specialty Packaging (%)

Soft caps

Caps

Tabs

Liquid

Other

64%

17%

14%

2%

2%

Raw materia!

TABLE3

Co-extractionmatrixProductiontechnologyBulk product

ColourViscositySpecificweight (20°):Composilion

LycopeneOtherCarotenoidsOthersconstituents:

E-vitamin (alfa-tocopherol,and the like):Other(tornato powder)

Tornato berries, produced aeeording to biologieregulation; non OGM berries; no peslicides andother phytomedicines and the like.Nuts, a!monds and the likeloily seeds,vegetables, other.Supereritical carbon dioxide extraction, by co-extraclion technologyFluid-oily suspension of Lycopene in natura!vegetable lipids, having characteristic smell.Dark redlbrown(Broockfield, R3, 20 rpm, 25° C.) 1500-3000 cPs0.928-0.948 kgll

1-2% (HPLCTitre)<2% (Lutein, Beta Carotene, Zeaxanthin, andthe like)Difference to 100%. Natural compounds,coming from the vegetable matrix and co-extracted with the Lycopene, as: phospholipids,poly-unsaturatcd fatty acids, tri-glycerides, di-glycerides, sterols, sterol esthers, sugars, otheranti-oxidant and the like0.2,0.5%

1-3%

25 TABLE4

Carotenoids Carotenoids percentage

30

Total Lycopene (cis + Irans)Total Beta-Carotene (cis + trans)LUlein (cis + trans)Other Carotenoids

82-88%3,6%2-3%

5-10%

TABLE535

Fattyacids Fatty acids percentage

40

Oleic acid (CI8:1)Linoleic acid (CI8:2)Linoleic acid (C 18:3)Palmitic acid (CI6:0)Stearic acid (CI8:0)Others

=80%=9%=1%=5%=2%=3%

45

What I claim is:1.A process for the co-extraction of organic lycopene from

tornato berries completely free ofpesticides, phytomedicinesand other toxic substances; said process is canied out withoutthe use ofharrnful and chemical solvents, using supercriticalcarbon dioxide, consisting 01' the following phases:

a) Vacuum dehydrating riddled tornato berries, by applyingcold or warm conditions, evaporating and sublimating;

b) Riddling and milling ofthe dry tornato benies until a finepowder is' obtained;

c) Mixing the obtained tornato powder with the same quan-tity ofa mixture 01' nut components selected from thegroup consisting of almonds, peanuts, walnuts, pista-chios;

d) Adding oily seeds, such as seeds selected from the groupconsisting of sunflower, soy, water melon, citrus fruits,pumpkin, grapefruit, and adding other vegetablesselected from the group consisting of rosemary, sage,oregano, garlic, carrots, cauliflowers, and adding fishmeal;

e) Milling and dehydrating said mixture unti! a homoge-neous paste is obtained;

f) Applying supercritical CO2, at a specific density, flowrate, pressure and temperature;

50

55

60

65

US 8,263,156 B29

g) Extracting lyc'opene simultaneously to the extraction ofother compounds, such as natural lipids, Lutein, Beta-Carotene, Zeaxanthin, E-vitarnin wherein said extractedlycopene has a 100% amorphous structure;

h) Mixture cooling;i) Pressure reducing;j) Collecting- the solution, which precipitates from the

mother solution;k) Further pressure reducing;I) Filtrating, condensing and collecting the solution in a

storage tank, including the CO2 recycling.

lO2. A process according to claim l,wherein said supercriti-

cal carbon dioxide pressure ranges between 400 and 600 bar.3. A process according lO claim l, wherein the supercritical

carbon dioxide temperature ranges between 320 and 3735 degrees Kelvin.

4. A process according to claim l, wherein said supercriti-cal carbon dioxide flow rate varies between 15 and 40 KgCOih.

5. A process according to claim l, wherein said supercriti-10 cal carbon dioxide density ranges between 0.8 and 0.95 kgll.

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