BR102017006947A2 - FRUIT JUICE PROCESSING - Google Patents

Abstract

The present invention relates to a method of producing a low-calorie fruit juice beverage, which may include passing a fruit juice stream containing unsweetened fruit juice components (product with fruit juice components) and sugars through a bed of resin. Due to the specific affinity of the resin for sugar, the fruit juice is chromatographically separated into concentrated product bands with fruit juice and sugar components, which move through the resin bed at different speeds. The concentrated band of sugar can be withdrawn as a sugar stream from a first extraction point in the resin bed, while the concentrated band of fruit juice components can be withdrawn as a product stream with fruit juice components. from a second extraction point different from the resin bed. The sugar stream includes a higher concentration of fructose, glucose and sucrose than the supply stream, while the product stream with fruit juice components includes a higher concentration of endogenous fruit juice compounds than the supply stream or the flow of sugar.

Description

FRUIT JUICE PROCESSING CROSS-REFERENCE TO RELATED ORDERS

[001] This patent application is, in part, a continuation under code 35 U.S.C. § 120 of U.S. Patent Application, no. 13/047,158, filed March 14, 2011, which is, in part, a continuation under code 35 U.S.C. § 120 of U.S. Patent Application, no. 11/881,364, filed July 26, 2007, which claims priority under code 35 U.S.C. § 365 for the International Patent Application, no. PCT/US2006/003149, filed January 27, 2006, which claims priority under code 35 U.S.C. § 119 for the U.S. Patent Application Temporary, no. 60/648,183, filed January 28, 2005, the contents of which are incorporated herein by reference.

BACKGROUND Technical Field

[002] The present invention relates to a method of selectively removing sugars (mixed sugars) from a fruit juice stream to produce a low-calorie fruit juice beverage which is nutritionally similar to natural juice.

Description of the Related Technique

[003] A juice is a natural fluid directly extracted or squeezed from a vegetable, such as a fruit. A product (e.g. a beverage) consisting of directly extracted or squeezed juice is considered 100 percent juice and may be declared as "100 percent juice." On the other hand, a "juice beverage" is defined as a juice drink product which contains juice but is less than 100% juice and more than 1% juice.

[004] The US Food and Drug Administration (FDA) calculates the percentage of juice when using a concentrate such as the minimum Brix levels listed below for natural juice (100 percent).

[005] Apple juice 11.5 Brix

[006] Grape juice 16.0 Brix

[007] Orange juice 11.8 Brix

[008] Pineapple juice 12.8 Brix

[009] According to the FDA, "if the nutrient profile of the juice has been lowered to a level below its normal range of nutrients" this means that that juice, to which such an important modification has been made, should not be included in the declaration of juice in total percentage" (21 C.F.R. §§101.30 &102.33).

[0010] Juices are an excellent source of vitamins, minerals and other beneficial compounds. However, an 8-ounce (240 ml) glass of orange juice, for example, contains 110 calories, which are primarily from the 22 grams of sugar. A glass of orange juice has about the same sugar and calorie content as a can of soda. And the US obesity and diabetes landscape is moving consumers toward lower-sugar, lower-calorie beverages. Although juice products have a high nutritional value, there has been a decline in juice consumption due, in part, to its relatively high calorie and sugar content. The low-calorie juice drinks currently available are primarily diluted juices (juice drinks) with juice flavoring and do not contain all the nutritional benefits of natural whole juice.

[0011] Orange juice, like most fruit juices, is defined and regulated according to its identification standard, which is based on the Brix value (soluble solids; which includes fructose, sucrose and glucose) of the juice. "Brix" is a refractive index scale for measuring the amount of sugar in a solution at a given temperature. Orange juice is conventionally produced by squeezing the liquid contents of ripe oranges. The resulting juice is then typically passed through a centrifuge or subjected to other processes to remove small pieces of orange peel and excess pulp.

[0012] Orange juice concentrate is produced by passing the final juice through a heat exchanger to remove most (about 75% to about 90%) of the original water. Orange juice concentrate is stored in frozen form for the required time. Frozen concentrate is transported domestically and internationally to local and regional beverage plants where it is reconstituted (water is returned to concentrate) to produce "orange juice" (100% orange juice; based on identification standard) and " orange juice drinks" (less than 100% orange juice; based on identification standard). This juice concentration process requires a high degree of energy and therefore can be costly. Storage and transport of frozen concentrate can also be costly due to its bulk.

[0013] Orange juice is also sold as a natural product and is labeled in the retail market as "non-concentrate orange juice". This product is typically sold at a higher than usual price because of its superior quality, additional storage, shipping cost (natural versus concentrate), and special (more onerous) storage requirements.

[0014] U.S. Patent, no. US-A-5,403,604 (Black) describes passing fruit juices through two membrane filtration systems. The separation process is based on molecular size and is not a selective sugar removal process. The first stage involved passing fruit juice through an ultrafiltration membrane. The retentate contained water, cloud oil, oil-soluble flavors, oil-soluble colors, and pulp. The permeate contained water, minerals, sugar and other lower molecular weight beneficial compounds. The permeate was subsequently passed through a nanofiltration membrane. The retentate contained water, sugar and other beneficial medium molecular weight compounds, while the permeate contained water, minerals and other low molecular weight compounds. The two membrane filtration processes resulted in the division of the juice into three molecular weight fractions (high, medium and low). The retentate from the first filtration (high molecular weight fraction) was then combined with the permeate from the second filtration (low molecular weight fraction) to produce a fruit juice with a low B/A ratio (Brix and acidity ratio). However, the low B/A product is devoid of the median molecular weight fraction. As a consequence according to the FDA, "if the nutrient profile of the juice has been lowered to a level below its normal nutrient range", it means that that juice, to which such an important modification has been made, should not be included in the total percentage juice claim" and would not meet the legal definition (identification standard) of a fruit juice or a fruit juice beverage.

[0015] U.S. Patent, no. 6,299,694 (Ma) describes the separation of an aqueous solution of fructose and glucose into a fructose peak and a glucose peak. The solution contained purified, ion-free water and two monosaccharides (carbohydrates) that have the same molecular formula (C6H12O6, MW 180.15), but with glucose having a six-membered ring structure and fructose having a six-membered structure. ring with five elements. The solution was passed through a resin exchange column to split the sample into two individual sugar peaks. Calcium from the calcium resin complex is attracted to the hydroxyl (OH) group of the sugar molecule. The fructose and glucose molecules in distilled water have different binding constants with the calcium resin complex. The difference in binding constants was used to separate fructose and glucose. The peaks comprised an ion-free aqueous glucose peak and an ion-free aqueous fructose peak. Ma teaches that the limitation presented by a resin consists in the fact that the aqueous solution containing sugars and water needs to be pure (free of contaminants) and "free of ionic substances that would impair the sorption capacity" of the resin to chromatographically separate the two sugars . Ma separates fructose and glucose, but does not mention how other sugars, sugar-containing compounds, or other compounds with hydroxyl (OH) groups would interact with the resin. Ma teaches from the combination of adding a sample that contains ions and contaminants to the column.

[0016] Those skilled in the art will readily understand that chromatography is a very rigorous science and that subtle changes in methodology, e.g. pH, free of ions, endogenous contaminants (pectin, pulp, dyes, sugars, etc.), will change the binding constant of fructose and glucose with the calcium resin complex. In addition to flow rate, sample size, sample preparation, ionic strength, polarity, etc. can alter the chromatographic separation of the sample. The chromatographic separation of a solution of pure water and two pure carbohydrates versus a sample containing a complex mixture of chemically dissimilar compounds is entirely different. (see C.F. Poole, "The Essence of Chromatography", Elsevier Science B.V., 2003).

[0017] Fruit juices contain significant amounts of unique ions. "Dionex Company" shows the ion concentration in a variety of fruit juices (eg orange juice, peach nectar, pear nectar, mango nectar and other fruit juices). For example, orange juice contains sodium (3 mg/L), potassium (1843 mg/L), magnesium (166 mg/L) and calcium (71 mg/L). In particular, the chemical composition of orange juice includes 76% carbohydrates (pulp, pectin, sugars), 9.6% acids, 5.4% free amino acids, 3.2% ions, 2.5% vitamins, 1.2% lipids, 0.8% flavonoids, 0.38% volatile and other non-volatile compounds, 0.013% carotenoids and enzymes.

[0018] Conventionally, it is difficult to reduce the amount of sugar in juices without also reducing the nutritional component thereof. As a result, most low-calorie juice products on the market are diluted fruit juices (juice drinks). In this regard, a variety of commercially available orange juices are supplemented with extra minerals (i.e. calcium) to meet consumer demands.

SUMMARY

[0019] A method of producing a low-calorie fruit juice beverage which retains most of the nutrients in the whole juice includes passing a supply stream of a fruit juice through a bed of resin. Fruit juice includes a product with unsweetened fruit juice components (hereinafter "juice component product" or "JCP") and sugar. As used herein, unsweetened fruit JCP includes unsweetened endogenous compounds such as parent ions, pectin, flavor compounds, aroma compounds, etc. The resin has a higher affinity for sugar than most products with juice components. However, the resin has a relatively weak attraction for sugars (eg, through weak linker complex). The resin can include calcium ions which form a calcium resin complex and have an attraction with the hydroxyl (OH) functional groups only sugar and other fruit juice molecules.

[0020] The method may further include chromatographically separating the fruit juice into concentrated product bands with fruit juice and sugar components that move through the resin bed. The concentrated sugar band moves along the resin bed at a slower rate than the concentrated product band with fruit juice components due to the relatively weak attraction between the resin and the hydroxyl functional group of the sugars. As a consequence, fruit juice can be separated into concentrated product bands with fruit juice and sugar components by means of the difference in the binding constants of the sugars with the resin complex.

[0021] The method may also include withdrawing the concentrated sugar band as a sugar stream from a first extraction point in the resin bed. The sugar stream can include a mixture of various sugars, such as a mixture of fructose and glucose, a mixture of fructose and sucrose, a mixture of sucrose and glucose, or a mixture of sucrose, glucose and fructose (depending on the type of fruit juice). fruit).

[0022] The method may also include withdrawing the concentrated band of product stream with juice components from a second extraction point in the resin bed. The second extraction point can be downstream of the first extraction point. The product stream with juice components includes a higher concentration of original free ions, pectin, flavor compounds and aroma compounds than either the supply stream or the sugar stream. The product stream with juice components also includes a higher concentration of endogenous flavor compounds, endogenous flavor compounds, endogenous acids, endogenous minerals, and endogenous vitamins than either the supply stream or the sugar stream. On the other hand, the sugar stream includes a higher concentration of fructose, glucose and/or sucrose than either the supply stream or the product stream with fruit juice components.

[0023] The product flow with fruit juice components is removed from the resin bed before the sugar flow. The first extraction point can be positioned axially so that a peak of the concentrated sugar band is drawn from the resin bed with the sugar flow. On the other hand, the second extraction point can be positioned axially so that a peak of the concentrated band of product with juice components is withdrawn from the resin bed with the flow of product with fruit juice components.

[0024] The fruit juice is not subjected to a deionization process before passing through the resin bed. The fruit juice can be one or more of: orange juice, cranberry juice, grape juice, apple juice, pineapple juice, tangerine juice, grapefruit juice, pomegranate juice, cherry juice, cranberry juice or strawberry juice. When the fruit juice is an orange juice, the orange juice may contain less than 15% by weight of pulp (e.g. less than 5 w/w%).

[0025] The method may also include adding a chelator to the fruit juice to bind the original free ions and protect against a shift of metal ions in the resin when the supply flow passes through the bed. The chelator can be added to fruit juice in a concentration of up to 20 w/w % (eg less than 2 w/w %). The chelator can be in the form of an acid or a salt. For example, the chelator can be at least one of ethylenediaminetetraacetic acid (EDTA) and ascorbic acid.

[0026] The method may also include concentrating the product stream with fruit juice components. The product stream with fruit juice components can be concentrated from 10% to 90% or more. This concentrate results in a significant volume reduction compared to standard juice concentrates due to reduced sugars. The processing cost of juice concentration is also significantly reduced due to the reduced concentration of sugars in the product stream with fruit juice components. Product concentrates with fruit juice components can result in significantly less frozen shipping and frozen storage costs compared to standard concentrates due to lower volume. Degradation of temperature, flavor and nutritional value of the juice is also reduced, as the concentration process requires less heat and time.

[0027] The method may also include adding a sweetener to the product stream with juice components to produce a low-calorie fruit juice drink. The sweetener can be at least one of a high intensity natural sweetener or a high intensity artificial sweetener. The high intensity natural sweetener can be stevia. The high intensity artificial sweetener can be at least one of sucralose, aspartame, acesulfame potassium, alitame, cyclamates and saccharin.

[0028] A method of producing a low calorie fruit juice drink may also include passing a stream of fruit juice (containing original free ions, pulp, pectin, flavor oils, acids, minerals, a chelator and other endogenous compounds ) in contact with a bed of ionic material capable of chromatographically separating the fruit juice within a "product with juice components" peak from the sugar peak (fructose, glucose and sucrose or fructose and glucose). Product spike with fruit juice components can be used to produce a product that would meet the identification standard for a "fruit juice drink". The original free ions are known to interfere with the chromatographic separation of the sample. The resulting product stream with fruit juice components exits the column before the mixed sugar peak. Process parameters such as depulping, pectin removal, addition of ions (cations, anions), flow rate, sample size, column diameter, column height (bed height) and pH of the fruit juice sample were modified to test various assumptions and to facilitate fractionation of the fruit juice sample into a product peak with fruit juice components and a sugar peak. A chelator can be added to the sample and/or eluent. The chelator would bind the free ions and thereby protect the calcium resin complex.

[0029] An organoleptically acceptable "fruit juice drink" can be produced from the product stream with fruit juice components by adding a high-intensity natural and/or artificial sweetener (e.g., sucralose, aspartame, saccharin , stevia or similar). By adding a low-calorie sweetener, a low-calorie "fruit juice drink" is produced. This drink will have most of the nutritional benefits of the original fruit without all of the original fruit calories, as a considerable amount of the sugar has been removed. It should be understood that other ingredients may also be added to the beverage (eg flavourings, pectins, minerals or the like) and that not all sugar needs to be removed from the beverage.

BRIEF DESCRIPTION OF THE DRAWINGS

[0030] The various features and advantages of the non-limiting embodiments presented herein will become more apparent upon review of the following detailed description, in conjunction with the accompanying drawings. The attached drawings are provided for illustrative purposes only and are not to be construed as limiting the scope of the claims. The attached drawings are also not to be considered as illustrations made to scale unless this is explicitly stated. For clarity, several dimensions of the drawings may have been enlarged.

[0031] Figure 1 is a schematic view of a system for chromatographically separating a supply stream (fruit juice) contained within a product spike with unsweetened fruit juice components and a sugar spike according to exemplary embodiments .

[0032] Figure 2 is a graphic illustration of a chromatographic separation performed by the system of figure 1.

[0033] Figure 3 is a graph of the results of a chromatographic separation of a simulated fruit juice solution of fructose and dye according to exemplary embodiments.

[0034] Figure 4 is a graph of the results of a chromatographic separation of apple juice according to exemplary embodiments.

[0035] Figure 5 is a graph of the results of a chromatographic separation of Concord grape juice according to exemplary embodiments.

[0036] Figure 6 is a graph of the results of a chromatographic separation of orange juice according to exemplary embodiments.

[0037] Figure 7 is a graph of the results of a chromatographic separation of orange juice with a chelator, according to exemplary embodiments.

DETAILED DESCRIPTION

[0038] It should be understood that when an element or layer is referred to as being "over", "connected to", "coupled to", or "covering" another element or layer, that element or layer may be directly over, connected a, coupled to or covering the other element or layer or intermediate elements or layers may be present. On the other hand, when an element is referred to as being "directly on", "directly connected to", or "directly coupled to" another element or layer, there is no intervening element or layer present. Like numbers refer to like elements throughout the specification. As used herein, the term "and/or" includes any and all combinations of one or more of the listed and associated items.

[0039] It should be understood that although the terms first, second, third, etc. are used herein to describe various elements, components, regions, layers and/or sections, those elements, components, regions, layers and/or sections shall not be limited by these terms. These terms are used only to distinguish one element, component, region, layer or section from another region, layer or section. Thus, a first element, component, region, layer or section discussed below could be termed as a second element, component, region, layer or section without deviating from the teachings of exemplary embodiments.

[0040] Spatially relative terms (eg, "below", "below", "inferior", "above", "superior" and the like) may be used here to facilitate the description of an element or characteristic relationship with another element (s) or feature(s) as illustrated in the figures. It should be understood that the spatially relative terms are intended to encompass different orientations of the device in use or operation, in addition to the orientation illustrated in the figures. For example, if the device in the figures is inverted, elements described as being "below" or "underneath" other elements or features would then be oriented "above" other elements or features. Thus, the term "below" can encompass both an orientation above and below. The device may be otherwise oriented (rotated by 90 degrees or other orientations) and the spatially relative terms used here interpreted accordingly.

[0041] The terminology used here is intended simply to describe the various modalities and not to limit exemplary modalities. As used herein, the singular forms "a", "an", and "the", "the" also include the plural forms, unless the context clearly indicates otherwise. It will also be understood that the terms "includes", "which includes", "comprises" and/or "comprising", when used in this specification, specify the presence of the characteristics, integers, steps, operations, elements and/or components mentioned, but do not preclude the presence or addition of one or more characteristics, integers, steps, operations, elements, different components and/or groups thereof.

[0042] Exemplary modalities will be described here with reference to cross-sectional illustrations, which are schematic illustrations of the idealized modalities (and intermediate structures) of the exemplary modalities. Therefore, variations in the formats of the illustrations as a consequence, for example, of manufacturing techniques and/or tolerances, must be assumed. Thus, the exemplary embodiments should not be interpreted as being limited to the shapes of the regions illustrated here, as they also include deviations in shapes from, for example, manufacturing. The regions illustrated in the figures are schematic in nature and their shapes are not intended to illustrate the actual shape of a region of a device and are not intended to limit the scope of exemplary embodiments.

[0043] Unless otherwise defined, all terms (which include technical and scientific terms) used herein have the same meaning as commonly understood by a person skilled in the art to which the exemplary embodiments belong. It will also be understood that terms, including those defined in commonly used dictionaries, are to be interpreted as having a meaning consistent with their meaning in the context of the relevant art and will not be interpreted in an idealized or overly formal sense, unless expressly defined. that way here.

[0044] Figure 1 is a schematic view of a system for chromatographically separating a supply stream (fruit juice) according to exemplary embodiments. With reference to Figure 1, a supply stream 10 of a sugar-containing liquid (eg fruit juice) is introduced into a column 12 containing a bed of resin. The supply stream 10 may be a fruit juice stream or other suitable composition stream. In an exemplary embodiment, the feed stream 10 is pre-treated before being introduced into the column 12. For example, the feed stream 10 may be subjected to centrifugation, filtration (e.g., hollow fiber filter) and/or other operations to remove most of the pulp, to remove some of the pectin, to remove acids, to add ions (cations, anions) and/or to adjust the pH to facilitate chromatographic separation from the feed stream 10. A chelator also can be added to supply stream 10 and/or eluent stream 14. The chelator acts to bind free ions from the supply stream 10, which protects the resin in the column 12 and improves the chromatographic separation of the supply stream 10. Chelators Suitable compounds include ethylenediaminetetraacetic acid (EDTA) and/or ascorbic acid, although exemplary embodiments are not limited thereto. A chelator can be present in a concentration ranging up to 20 w/w%. For example, a chelator can be present at a concentration between 0.0001 to 5 w/w % (eg, 0.1 to 2 w/w %).

[0045] After pretreatment, the supply stream 10 enters the top of column 12 and passes through a bed of resin (for example, a simulated moving bed of resin granules) to the bottom of column 12. The circulation of supply flow 10 through column 12 may be gravity driven or pressure driven. The resin is an ion exchange resin that has an attraction for sugars (eg, fructose, glucose) in supply stream 10. However, the resin does not capture or remove sugars from supply stream 10. Instead, the resin resin exhibits an attraction for the hydroxyl group (OH) on sugars. As a consequence, the sugars will continue to move through the resin bed with supply stream 10, but at a slower rate than the product with juice components of supply stream 10 (eg in the form of concentrated bands). The difference in binding constant with the resin complex of calcium and sugars is used to separate the individual sugars. With the proper combination of chromatographic process parameters, as will be discussed in more detail here, the supply stream 10 can be separated into a product stream with juice components 18 and a sugar stream 16. The sugar stream 16 is the residual flow from the chromatographic process. Suitable resins include Dowex® Monosphere® 99CA/320 separation resins (from Dow Chemicals, Midland, MI), although exemplary embodiments are not limited thereto.

[0046] The (residual) sugar stream 16 is withdrawn from an upper extraction point of the column 12. The upper extraction point is below an inlet point, through which the supply stream 10 is introduced. Sugar stream 16 is a mixed sugar fraction in the sense that it includes a combination of fructose and glucose or a combination of at least fructose, glucose and sucrose. On the other hand, the product stream with juice components 18 is drawn from a lower extraction point in column 12. The product stream with juice components 18 has a higher concentration of ions, endogenous flavor compounds, endogenous aroma compounds , endogenous acids, endogenous minerals, endogenous vitamins and other endogenous compounds than sugar flow 16 (eg at least 45% greater, relative to the dry residue). On the other hand, the product stream with juice components 18 has a lower sugar content than the supply stream 10, while the sugar stream 16 has a higher sugar content than the supply stream 10. In a non-limiting example , sugar stream 16 includes at least 45% (e.g., at least 60%) of the sugars in supply stream 10 and not more than 35% (e.g., no more than 20%) of the unsweetened juice components in supply stream 10. The lower extraction point of the product stream with juice components 18 is below the upper extraction point of the sugar stream 16. In an exemplary embodiment, the product stream with juice components 18 has at least 45 % less sugar than in sugar stream 16. In a non-limiting example, product stream with unsweetened juice components 18 contains at least 65% of the unsweetened juice components in supply stream 10 and no more than 55% (e.g. no more than 35%) of the sugars in the f luxury of supply 10.

[0047] An eluent stream 14 (e.g. water stream) may be introduced into the column 12 to assist in separating the supply stream 10 into the product stream with juice components 18 and the sugar stream 16. recycle stream 20 can be employed to improve the efficiency of the chromatographic separation. In a non-limiting embodiment, the system of Figure 1 can be a simulated moving bed that performs the continuous process of taking a fruit juice supply stream and dividing it into a product stream with juice components and a stream of sugar. Although a single column is shown in figure 1, it should be understood that a plurality of columns (eg 2, 3 or more) may be used, either arranged in series, or in parallel, or in a combination of both options.

[0048] Figure 2 is a graphic illustration of a chromatographic separation performed by the system of figure 1. With reference to figure 2, the removal of the product stream with juice components 18 is done at a point in the column 12 at which the concentration of product with juice components is greater than supply flow 10 (for example, where the product concentration with juice components is in a high concentration range and the sugar concentration is in a lower concentration range). On the other hand, the removal of sugar stream 16 (e.g. sugar fraction) is done at a point in column 12 when the sugar concentration is greater than supply stream 10 (e.g. where the sugar concentration is in a maximum concentration range and where the product concentration with juice components is in a lower concentration range). The introduction of the supply stream 10 is located at the point in column 12 where the least amount of separation of the sugar stream 16 and the product stream with juice components 18 is occurring. The eluent stream 14 is introduced into column 12 after the sugar flow removal 16 to maintain mass balance and constant flow during recycling.

[0049] Column 12 may be in the form of a plurality of columns which are extended in series, in parallel, in cascade or the like for additional treatment time, for capacity or for special effects. In an exemplary embodiment, when orange juice is introduced as supply stream 10, the product fraction with orange fruit juice components that exits as product stream with juice components 18 will not meet the "juice" identification standard. juice", but could be used to produce a "fruit juice drink". Notably, the product stream with juice components 18 can be used to produce products that benefit both the consumer and the manufacturer.

chromatography

[0050] Those skilled in the art will readily understand that chromatography is a very rigorous science. Results can be very difficult/impossible to predict, as subtle changes in methodology (eg pH, free ions, change in binding constant of endogenous components to resin) can affect the success of the separation. In addition, factors such as flow rate, sample size, sample preparation, ionic resistance, polarity, etc. significantly alter the chromatographic separation of the sample and can be the difference between sample separation success and failure. A person skilled in the art will also understand that endogenous contaminants (eg, pectin, pulp, dyes, sugars or other compounds with hydroxyl (OH) groups, etc.) present in the sample may interfere with or impede the chromatographic process (eg, using if Dowex® Monosphere® 99CA/320 separation resin) from the sample. Contaminants can cover or adhere to active sites on the resin, can compete with the target compound of the active sites, clog the resin beads or column and/or degrade the resin beads, etc. Differences in chromatographic parameters can mean a difference in sample separation into clear individual compound peaks, a large broad peak with mixed compounds, an unidentified peak, or the complete inability to separate the sample.

[0051] The chromatographic separation between a solution of pure water and two pure carbohydrates and the chromatographic separation of a solution containing a complex mixture of peculiar chemical compounds (contaminants) are totally different. For example, fruit juices have a variety of endogenous compounds, which can interfere with the chromatographic separation of the juice. Endogenous compounds include, but are not limited to, pectin, pulp, flavor oils, dyes, sugars, etc.

[0052] Various minerals (eg, ions) can be added to the supply stream to bind to active sites of endogenous fruit juice compounds so as to reduce interaction with the resin.

[0053] Calcium, a divalent cation, is commonly added to a solution to increase thickness, form a gel, or flocculate suspended compounds. Calcium ions can also adhere to a physically immobile matrix. In such an example, one positive charge (from Ca+2) forms a bond with the matrix (eg, resin), while the other positive charge interacts with the other charged particles or hydroxyl group-containing particles. Calcium ions can be added to the solution to remove suspended particles by forming bonds between two suspended particles, resulting in a larger complex. As the particles increase in size, they fall out of solution.

[0054] The binding constant of the interaction between calcium ions and other particles determines the binding strength. Bond strength varies from weak, medium, and strong. Ionic bonds are electrovalent bonds that form from the electrostatic attraction between two oppositely charged ions (atoms). Ionic bonds transfer electrons from one ion to another to fill the valence shells. Covalent bonds are chemical bonds that form between two atoms where they share electrons and form shared full valence shells.

[0055] Fruit pectins (which includes citrus pectins) are used in the food industry as a gelling agent, thickener and an emulsifying agent. Fruit pectins are heterosaccharides and are divided, by their degree of esterification, into low-methoxy pectin and high-methoxy pectin. These two types of pectins form a gel with different mechanisms. Low methoxy pectins are used in the food industry to produce low sugar jams and jellies as they do not need sugar to create gels. However, low methoxy pectins need calcium (calcium reactivity) to produce a gel. High methoxy pectin, on the other hand, needs a high concentration of sugar to form a gel. Citrus pectins are known to react with calcium and produce strong, good quality gels.

[0056] Pectins are composed of long chains of sugar molecules. They are primarily composed of D-galacturonic acid (>74%) linked to α (1–4), but also contain rhamnose, arabinose, galactose, xylose, and other sugar molecules. The sugar molecules of pectin, as well as the fructose and glucose molecules contain hydroxyl (OH) functional groups, which are attracted to the calcium ions of the calcium-resin complex. The binding constants of the individual sugar molecules as well as the polysaccharides need to be determined to see how they react with the resin. Once the binding constants are determined, it is also necessary to determine how they will interact with the sugars (eg, glucose and fructose) during a chromatographic separation of the juice sample. At least the following possibilities exist:

[0057] 1. Pectin sugars will irreversibly bind calcium.

[0058] 2. Pectin sugars will be attracted by the calcium resin complex, but will not bind to the resin.

[0059] 3. Pectin will not have any interaction with the active site in the resin granules.

[0060] 4. On a physical level, pectin could also cover active sites without reacting with the active site, without clogging the resin granules and/or clogging the column.

[0061] Plant fibers are primarily composed of cellulose and semicellulose and are known to have some functional properties that include water holding capacity, viscosity, gel formation and dietary fiber with cation exchange capacity. Orange juice pulp is composed of non-starch polysaccharides, which include cellulose, (linear B(1-4) bonding chains of glucose molecules), semicelluloses, (linear B(1-4 bonding) chains and branched (α (1-3 bond)) of sugars that include glucose, xylose, mannose, galactose, rhamnose, arabinose, and lignin-crosslinked phenol polymers. Lignins are not composed of sugar molecules like cellulose and semicelluloses, but the monomers still contain hydroxyl groups (OH), which can be attracted by the Dowex® Monosphere® 99CA/320 separation resin.

[0062] Citrus oils (essential oils) are produced by citrus fruits in cells located in the peel of the fruit. Citrus juices that have flavoring oils include orange, tangerine, grapefruit, etc. The composition of flavoring oils varies according to the type of fruit and its variety. Orange flavor oils include hundreds of organic compounds as analyzed by gas chromatography. Most flavor compounds belong to the terpene family, which includes d-limonene. The other compounds include acids, aldehydes and alcohols, which include octanal, decanal and 1-octanol. Since aldehydes and alcohols also contain hydroxyl (OH) groups, they can be attracted to the resin (the resin complex is attracted to the hydroxyl group of fructose and glucose) and inhibit or interfere with the separation of sugars from fruit juice. Other compounds in citrus fruits may include pinene, sabinene, myrcene, linalool, carene, etc.

Benefits for the Consumer

[0063] A beverage containing product with components of fruit juice, water and a high-intensity natural and/or artificial sweetener (for example, sucralose, stevia or similar) produces a fruit juice beverage (which meets the standard identification) which is on par in terms of sensory evaluations with its standard juice equivalent. Notably, the fruit juice drink will have most of the vitamins, minerals, and other beneficial compounds in the fruit juice without all the calories in the sugar. Flavorings and other ingredients can be added to enhance the sensory characteristics of the fruit juice drink. Citrus pectin or some other carbohydrate (gummies, etc.) can be added to provide additional viscosity and the desired mouthfeel.

[0064] Juice consumption has declined, in part, due to the drink's relatively high calorie content. A lower calorie product will provide consumers with the opportunity to consume orange fruit juice beverages, using a product with orange juice components, with the benefits of "orange juice" and without worrying about the added calories of "orange juice". orange". In the present description, it should be understood that the terms "orange juice" and "orange juice concentrate" mean the standard for identifying the liquid contents extracted from oranges. Some of the benefits of this process for the consumer are as follows.

[0065] • Low calorie "Orange fruit juice drink"

[0066] • "Orange fruit juice drink" with little sugar

[0067] • "Orange fruit juice drink" with nutritional value similar to "orange juice", but without all the sugar or calories content

[0068] • Higher quality "Orange juice concentrates and beverages"

[0069] • Possibility of drinking more products containing "orange juice"

Benefits for the Manufacturer

[0070] The product with fruit juice components can be used to produce product concentrates with fruit juice components (for example, for fruit juice drinks), product flavorings with fruit juice components (for example, for beverages, etc.) and ingredient components for product with fruit juice components (eg, for candy, etc.). Conventionally, products containing sugar in a standard concentration can be relatively expensive due, in part, to their high sugar content, which results in high viscosity and high energy requirements. By using a product with fruit juice components (which contain a lower amount of soluble solids), the energy requirement for processing will be significantly reduced. Less energy is required to concentrate solutions with low soluble solids compared to high soluble solids solutions. These thermal processing savings can range from around 10% to around 50% or even more than that in the case of operating costs. The concentrate resulting from the product with fruit juice components can be recombined with water and a high intensity sweetener to produce low calorie beverages. In addition, storage and transport costs (frozen and refrigerated) of the product with fruit juice components for natural juice and concentrate are significantly reduced as a result of the reduction of sugar. This savings can range from around 10% to around 70% or even more than that.

[0071] Below are some of the benefits of this process for the manufacturer.

[0072] • Marketing a new "fruit juice drink" that is similar in nutritional value to standard "juice" but without all the sugar or calories

[0073] • The commercialization of a new low-calorie "fruit juice drink" with benefits for the consumer

[0074] • The commercialization of a new "fruit juice drink" with little sugar and benefits for the consumer

[0075] • Lower processing costs during the concentration process

[0076] • Lower frozen storage costs

[0077] • Lower frozen transport costs

[0078] • The commercialization of new products, such as, for example,

[0079] • Fruit-based drinks

[0080] • Low-sugar/low-calorie "Fruit Juice Drink" with high-intensity sweeteners

[0081] • Low-sugar/low-calorie "Fruit flavor"

[0082] • Low-sugar/low-calorie "Fruit Ingredient"

EXPERIMENTAL ANALYSIS

[0083] An experiment will be discussed here, which was divided into five trials. Each trial used an increasingly complex fruit juice. The first test involved separating a simulated juice from an aqueous fructose solution containing a blue dye into an aqueous blue dye solution peak (blue dye and distilled water) and an aqueous fructose solution peak (purified fructose and distilled water). ) using Dowex® Monosphere® 99CA/320 separation resin. The water was degassed, distilled, purified and freed from ions. Fructose has been freed from ions, purified and freed from contaminants. A number of parameters, which include sample size, column diameter, column height and flow rate were varied for testing and process determination. The sample size was evaluated from 10 ml to 40 ml. The diameters of two columns (1.9 cm and 3 cm) were investigated. Column height was studied in a range of 30 cm to 100 cm. The flow was studied from 1 ml per min to 10 ml per minute.

[0084] The second test involved separating an apple juice sample into an apple "product with juice components" peak (later "JCP") and a sugar peak using Dowex® Monosphere® 99CA separation resin /320. The apple juice sample contained free ions, pectin, fructose, glucose, sucrose, acids, flavor compounds, aroma compounds and other endogenous compounds (contaminants). Apple juice contains glucose (about 27%), fructose (about 60%) and sucrose (about 13%). Free ions are known to reduce chromatographic separation of the sample and pectins are very reactive with calcium. The resin used is calcium resin complex. It was not known how free ions, calcium sensitive pectins and endogenous compounds would affect the chromatographic process. The water was degassed, distilled, purified and freed from ions. A number of parameters, which include apple juice sample size, column diameter, column height, flow rate and pH were varied for process testing and determination. The apple juice sample size was evaluated from 10 ml to 40 ml. Column height was studied in a range of 30 cm to 100 cm. The flow was studied from 1 ml per min up to 10 ml per minute. The pH of apple juice was investigated from a pH of 2 to 6.

[0085] The third trial involved separating a sample of Concord grape juice onto a Concord grape JPC peak and a sugar peak using Dowex® Monosphere® 99CA/320 separation resin. The Concord grape juice sample contained free ions, pectins, dyes, fructose, glucose, acids, flavor compounds, aroma compounds and other endogenous compounds (contaminants). Concord grape juice contains glucose (about 48%), fructose (about 52%) and sucrose (less than 1%). Free ions are known to reduce chromatographic separation of the sample and pectins are very reactive with calcium. The resin used is calcium resin complex. It was not known how free ions, calcium sensitive pectins, dyes and endogenous compounds would affect the chromatographic process. The water was degassed, distilled, purified and freed from ions. Optimal process parameters (sample size, flow rate, column diameter and height) of the apple juice were used with the Concord grape juice sample. However, pH adjustment and ion addition were varied for process testing and determination.

[0086] The fourth test involved separating an orange juice sample into an orange JCP peak and a sugar peak using Dowex® Monosphere® 99CA/320 separation resin. This assay was designed to analyze the effect that a more complex fruit juice (with more pectin, pulp, flavoring orange oils and other contaminants) has on the chromatographic separation of an orange juice sample into an orange JCP peak and a sugar spike. Orange juice contains glucose (about 26%), fructose (about 28%) and sucrose (about 46%). The orange juice used in the trial was significantly more viscous (thicker) and had a higher concentration of complex mixtures of contaminants than the apple or Concord grape juice sample used in the second or third trials. The orange juice sample contained free ions, pulp, pectin, flavor oils, fructose, glucose, sucrose, acids, beta-carotene (colorant), flavor compounds, aroma compounds and other endogenous compounds (contaminants). Free ions are known to reduce chromatographic separation of the sample and pectins are very reactive with calcium. The pulp is composed of monomers with hydroxyl functional groups and can interact with the calcium resin complex. It was not known how free ions, a higher concentration of calcium-sensitive pectins, pulp, flavor oils, beta-carotene (color) and endogenous compounds would affect the chromatographic process. The water was degassed, distilled, purified and freed from ions. A number of parameters, which include orange juice sample size, column height, flow rate and pH were varied for testing and process determination. The orange juice sample size was evaluated from 10 ml to 40 ml. Column height was studied in a range of 30 cm to 100 cm. The flow was studied from 1 ml to 10 ml per minute. The eluent headspace has been increased to obtain the highest flow rates and largest sample size. The pH of orange juice was investigated from a pH of 2 to a pH of 6.

[0087] The fifth trial involved separating an orange juice sample with a chelator (eg, added EDTA) into an orange juice with an added EDTA JCP peak and a sugar peak using Dowex® Monosphere® separation resin 99CA/320. This assay was designed to evaluate the effect that a chelator added to the sample has on the separation of an orange juice sample into a chelated orange JCP peak and the sugar peak. The orange juice sample contained free ions, pulp, pectin, orange flavor oils, fructose, glucose, sucrose, acids, flavor compounds, aroma compounds and other endogenous compounds (contaminants). Orange juice contains glucose (about 26%), fructose (about 28%) and sucrose (about 46%). Free ions are known to reduce chromatographic separation of the sample and pectins are very reactive with calcium. Endogenous compounds with hydroxyl groups can interact with the resin. The resin used is calcium resin complex. It was not known how the addition of a chelator would affect the chromatographic process. The water was degassed, distilled, purified and freed from ions. As noted above, a chelator (eg EDTA) was added to the orange juice sample. The chelator was added to bind free ions, reduce free ion concentration, and/or to make free ions less reactive. Upon being chelated, the free ions are no longer able to dissociate calcium from the calcium-resin complex, thereby protecting the calcium-resin complex. Otherwise, dissociation of calcium from the calcium-resin complex would render the resin incapable of chromatographic separation of the sample. The optimal parameters from the fourth trial (orange juice) were used for the chelating orange juice (eg, EDTA) from the fifth trial.

EXPERIMENTAL PROCEDURE Resin Conditioning

[0088] The separation resin Dowex® Monosphere® 99CA/320 (Supelco Inc.) was conditioned by transferring the new wet resin to a glass container with degassed and distilled water. The distilled water was degassed using a vacuum for 24 hours with intermittent stirring of the liquid before use. The resin was slowly mixed into 4 volumes of degassed and distilled water (ion-free) at room temperature and stored overnight. After 12 hours of conditioning, the resin was gently stirred and allowed to settle for 3 minutes before the supernatant was decanted to remove fine particles. The resin was washed with 3 volumes of degassed and distilled water, set aside for 3 minutes and the supernatant was decanted. The procedure was repeated three times until the supernatant was clean and free of fine particles, at which point the resin was considered conditioned.

Column Preparation

[0089] Fifty milliliters of degassed and distilled water were added to the column. A plastic screen was placed at the bottom of the column outlet tube to prevent resin from clogging the outlet tube. The distilled water was degassed using a vacuum for 24 hours with intermittent stirring of the liquid. The conditioned separation resin slurry Dowex® Monosphere® 99CA/320 was added to the column containing degassed and distilled water. The eluent flow rate was maintained throughout the addition to obtain a packed column of homogeneous. The concentration of the resin slurry was also maintained during pouring to obtain a homogeneous density in the packed column. The column was devoid of "drip layers" or high and low density pockets within the column which would alter the sample chromatography. The water level was maintained above the resin surface throughout this pouring process. The height of the final resin bed was 63.5 cm with a diameter of 3 cm. A circular plastic screen was placed on the surface of the resin in the column. Circular plastic screen is added to reduce agitation in the resin bed when sample is applied.

[0090] A test solution (blue dye and distilled water) was applied to the column and eluted through the column to test the homogeneity of the resin bed. As the blue color moved through the bed, "layers" and "dense and less dense" spots were shown within the column. Columns with irregularities were not used, as irregularities interfere with sample elution. In addition, columns that developed air bubbles before or during sample separation were dismantled and the resin reconditioned, as air bubbles interfere with sample elution. Also, in cases where the bed height increased or decreased, the results were discarded and the test was repeated with a new column. Also, in cases where the flow rate significantly increased or decreased during the run, the results were discarded and the run was repeated with a new column.

Sample Preparation

[0091] Five samples were prepared: 1) simulated juice, 2) apple juice concentrate, 3) Concord grape juice concentrate, 4) orange juice concentrate, and 5) orange juice concentrate with a chelator (for example, EDTA). None of the juice concentrates were treated to remove the original free ions.

[0092] The first sample was a simulated juice containing a fructose solution (a simple carbohydrate and a distilled water solution) with a blue dye. The simulated juice was developed to simulate a simple juice, purified and free of contaminants, without ions, pulp, pectin, flavoring oils, dyes, acids, glucose, sucrose flavor compounds, aroma compounds or other matter (contaminants) that interfere with the chromatographic separation. The solution was prepared by combining 144 gm of purified crystalline fructose; 200 ml of degassed and distilled water at room temperature (ion-free) and a drop of blue color (Mcormick Neon Food Colors). The solution was manually stirred until the crystalline fructose was dissolved without incorporating air into the sample. The resulting solution had a Brix value of 42.3˚ as measured with a portable refractometer (Epic Inc., 30% 60%). All measurements of Brix values in this assay were incorrect for acid. The pH of the solution has not been adjusted. The sample was degassed under a vacuum for 2 hours before use. The column, eluent and sample were brought to room temperature before the sample was applied to the column.

[0093] The second sample was from an apple juice concentrate. Apple juice was evaluated to verify if a complex sample of fruit juice containing free ions, pectin, fructose, glucose, sucrose, brown dye (phenolic compounds oxidized by polyphenol oxidase enzyme), acids, flavor compounds, aroma compounds and other endogenous compounds (contaminants) could be chromatographically separated into an apple JCP peak and a sugar peak. The apple juice sample was prepared by combining apple juice concentrate at room temperature (Langers 100% apple juice) and degassed and distilled (ion-free) water at room temperature. The apple juice concentrate and distilled water were stirred to produce a homogeneous sample without incorporating air into the sample. The concentrate was diluted with water as the apple juice concentrate was too viscous. The initial Brix value of the apple juice sample was determined to be about 50˚ Brix as measured with a portable refractometer (Epic Inc. 30% 60%). The apple juice sample was divided into three hundred ml aliquots and the pH of the samples was adjusted. Once the pH was adjusted, degassed and distilled water was added to the apple juice sample to obtain a value of 42.3 Brix. A pH range of apple juice solutions was evaluated during chromatographic separation of the apple juice sample. Samples were degassed under a vacuum for 2 hours before use. The column, eluent and samples were at room temperature before the sample was applied to the column.

[0094] The third sample was from a Concord grape juice concentrate. Concord grape juice was evaluated to see if a more complex sample of fruit juice containing free ions, pectin, dyes, fructose, glucose, acids, flavor compounds, aroma compounds and other peculiar endogenous compounds (contaminants) could be chromatographically separated into a peak of Concord grape juice JPC and a peak of sugar. Concord grape juice contains fructose, glucose and may have an identifiable amount of sucrose. Concord grape juice also has different endogenous compounds compared to apple juice. The sample was prepared by combining Concord grape juice concentrate (Welch, 100% grape juice) (64˚ Brix) that was at room temperature with degassed and distilled (ion-free) water. The combination was agitated to maintain a homogeneous sample without incorporating air into the sample. The diluted Concord grape juice sample was divided into 300 ml aliquots and the pH was adjusted. Once the pH was adjusted, degassed and distilled water was added to the orange juice sample to obtain a value of 42.0 Brix, measured with a portable refractometer (Epic Inc., 30% 60%). A pH range of Concord grape juice solutions was evaluated to see if they would affect the chromatographic separation of the Concord grape juice sample. The sample was degassed under a vacuum for 2 hours before use. The column, eluent and samples were at room temperature before the sample was applied to the column.

[0095] The fourth sample was from a clarified orange juice concentrate. Orange juice was evaluated to see if a more complex and more viscous sample of fruit juice containing more pulp and pectin, free ions, flavor oils, acids, flavor oils, flavor compounds and other endogenous compounds (contaminants) could be chromatographically separated into an orange JCP peak and a sugar peak. Orange juice contains peculiar endogenous compounds compared to apple and Concord grape juice.

[0096] Initially, a low-pulp orange juice concentrate was diluted with degassed and distilled water, mixed and passed through a filter to produce a low-pulp, pectin orange juice sample. However, the orange juice sample was too thick and the process was unsuccessful.

[0097] Next, commercially available pulpless orange juice concentrates were evaluated. The sample was diluted in degassed and distilled water, mixed, filtered and applied to the column. However, the diluted orange juice sample clogged the column. Commercial orange juice without pulp was diluted in natural juice (11.8 Brix) and evaluated in the column. The natural juice did not clog the spine and passed through it easily. However, the resulting fractions were too diluted to be properly evaluated.

[0098] After the first two tests, it was observed that the resin was being damaged by the orange juice concentrates. A dilute solution of orange oils was mixed with the resin overnight and evaluated. The resin was damaged by the orange oils and, as a result, subsequent orange juice concentrates were added without flavoring (no orange oils) back into the juice.

[0099] Next, a clarified concentrate (passed through a membrane filtration system) of commercially available orange juice, with no flavoring added back (no flavoring oils), was evaluated. However, the juice concentrate was too thick to apply directly to the column. As a consequence, the juice was brought to room temperature, diluted in water and then applied to the column. Furthermore, with an increase in the eluent headspace (increased column pressure), the sample passed through the column. Clarified orange juice was subsequently used in the assays.

[00100] The sample for the fourth test was prepared by combining a clarified orange juice concentrate (reduced pulp and pectin) (68.2˚ Brix) (Cargill Inc.) and degassed and distilled water (free of ions). The combination was agitated to maintain a homogeneous sample without incorporating air into the sample. The diluted orange juice sample was divided into 300 ml aliquots and the pH was adjusted. Once the pH was adjusted, degassed and distilled water was added to the orange juice sample to obtain a value of 42.0 Brix, measured with a portable refractometer (Epic Inc., 30%-60%). A pH range of orange juice solutions was evaluated to see if they would affect the chromatographic separation of the orange juice sample. The sample was degassed under a vacuum for 2 hours before use. Five hundred ml of warm degassed and distilled water (80-85°F) was passed through the column to increase the column temperature. The sample was heated to 80-85°F to reduce its viscosity before being applied to the column. The eluent was also heated to 80-85°F.

[00101] The fifth sample was from a clarified orange juice (no flavoring added back) with an added chelator (eg EDTA). Orange juice with EDTA was evaluated to see if adding EDTA to a complex and viscous sample of fruit juice containing high concentrations of pulp, pectin, free ions, flavor oils, beta-carotene (color), flavor compounds, aroma and other endogenous compounds (contaminants), the clarified orange juice could be chromatographically separated into an EDTA orange JCP peak and a sugar peak. EDTA was added to orange juice to bind free ions. The sample was prepared by combining a concentrate (pulp and pectin reduced) of clarified orange juice (no flavoring added back) (Cargill Inc.) with degassed and distilled water at room temperature, and the combination was shaken to maintain a sample homogeneous without incorporation of air to the sample. Orange juice concentrate (68.2˚ Brix) was also diluted in degassed and distilled water to reduce its viscosity. The diluted orange juice sample was divided into 300 ml aliquots, the EDTA was added and the pH was adjusted. EDTA was in acid form. Once the pH was adjusted, distilled water was added to the orange juice sample to obtain a value of 42.0 Brix, measured with a portable refractometer (Epic Inc., 30% 60%). A pH range of orange juice with EDTA solution was evaluated for the analysis of the effect it would have on the chromatographic separation of the sample. The sample was degassed under a vacuum for 2 hours before use. Five hundred ml of warm degassed distilled water (80-85°F) was passed through the column to increase the column temperature. The sample was heated to 80-85°F to reduce sample viscosity before being applied to the column. The eluent was also heated to 80-85°F.

EXPERIMENT RESULTS Simulated Juice Results

[00102] In the first test, the objective was to chromatographically separate a simulated juice, composed of an aqueous solution of fructose (simple carbohydrate solution) and a blue color sample, into a peak of aqueous blue color and a peak of aqueous fructose ( sugar). Fructose has been freed from ions, purified and freed from contaminants. The results showed the simulated juice splitting into a semi-blunt blue colored peak and a semi-broad fructose peak. A series of chromatographic parameters were evaluated (column diameter, sample size, flow rate and column height (bed)) to optimize the process.

[00103] The diameters of the columns (1.9 cm and 3 cm) were evaluated for the separation of the simulated juice solution. The column with the smallest diameter (1.9 cm) exhibited sharper peaks, but the sample size was too small to analyze (quantitatively) for the blue peak. As a consequence, all other tests were conducted with the larger diameter column (3 cm).

[00104] The sample size was evaluated from 10 to 50 ml. The smaller size sample (10 ml) did not show good visual results of the blue colored peak. The larger size sample with high flow rate resulted in a large and broad chromatographic peak. However, medium and large size samples with medium flow rate produced good peaks.

[00105] The heights of the columns (bed) were evaluated from 40 cm to 100 cm. The smaller column did not produce good separation of the blue colored peak and the fructose peak. The 100 cm high flow rate column produced large and broad blue and fructose peaks. Medium and large sample sizes and medium and tall columns with medium flow rate produced good peaks. Small sample sizes, medium and large column heights, and high flow rates produced very dilute samples. Furthermore, the blue color peak was wide and the color was too light to quantify. The ideal bed height was 63 – 100 cm, which produced separate and distinct peaks.

[00106] Flow rates have been rated from 1 to 10 ml per minute. The slower flow rate was too slow and the chromatography took too long. The fastest flow rates were too fast and distorted the chromatographic peaks. The ideal flow rate was 3.7-6.0 ml per minute

[00107] Figure 3 is a graph of the results of a chromatographic separation of a simulated juice solution according to exemplary modalities. Referring to Figure 3, the simulated juice solution was chromatographically separated into two peaks. The first peak was composed of the blue colored solution and the second peak was a sugar peak (fructose peak). The blue color exited the column in a well-defined bell-shaped curve, while the fructose produced a positively oblique curve. Tubes 3 and 4 had the maximum blue color (visual), while tube 9 had the highest Brix value, as measured with a portable refractometer (Reichert model 10430 0-30 Brix). The assay was performed in triplicate and obtained good reproducibility. The average of the three data sources is shown below in Table 1.

Apple Juice Results

[00108] In the second test, the objective was to chromatographically separate an apple juice sample into an apple JCP peak and a sugar peak. The results showed a sample separation of apple juice that contained free ions, pectin, fructose, glucose, sucrose, acids, flavor compounds, aroma compounds and other endogenous compounds (contaminants) within a semi-sharp peak of apple JCP and a semi-wide peak of sugar (fructose, glucose and sucrose). A number of chromatographic parameters were evaluated, which include sample size, flow rate, column height (bed) and pH.

[00109] The sample size was evaluated from 10 to 50 ml. The smallest sample size (10 ml) did not exhibit good apple JCP peak visual or sensory results. Medium and large sample sizes with medium flow resulted in good apple JCP peaks.

[00110] Column (bed) heights were evaluated from 40 cm to 100 cm. The shorter column did not produce a good separation of apple JCP peak and sugar peak. Medium and taller columns with medium sample size produced good peaks. The ideal bed height was 63-100 cm, which produced separate and distinct peaks.

[00111] Flow rates have been rated from 1 to 10 ml per minute. The slower flow rate was too slow and the chromatograms took too long. The faster flow rates were too fast and distorted both chromatographic peaks. Medium and large sample sizes and medium and high columns with medium flow rate produced good peaks. Based on the results, it was found that the ideal flow rate is 3.7 – 6.0 ml per minute.

[00112] The pH of the apple juice samples was evaluated from 2 to 6. The pH of the sample affected the separation of the apple juice sample and the chromatographic formats of the apple JCP peak and the sugar peak.

[00113] Figure 4 is a graph of the results of a chromatographic separation of apple juice according to exemplary modalities. With reference to Figure 4, the apple juice is separated into two chromatographic peaks. The first peak was composed of the apple JCP peak and the second peak was a sugar peak (fructose, glucose and sucrose). Although the apple juice sample contained significant amounts of free ions, pectin, glucose, sucrose, flavors, acids, and other endogenous compounds (contaminants), it was separated into an apple JCP peak and a broad sugar peak. In particular, sugars (eg fructose, glucose, sucrose) eluted in a single peak rather than individual sugar peaks. In addition, the apple JCP peak eluted about 10 ml later than the blue colored peak from the first run (dummy juice) above due to contaminants in the apple juice sample. The contaminants interfered with the chromatographic separation of the sample. The apple JPC produced a well-defined bell-shaped curve, while the sugar peak (fructose, glucose, sucrose) produced a positively slanted curve. Tube 4 had the maximum color, acidity and flavor (sensory evaluation), while tube 9 had the highest Brix value, as measured with a portable refractometer (Reichert model 10430 0-30 Brix). The assay was conducted in triplicate and showed good reproducibility. The average of the three data sources is shown below in Table 1.

Concord grape juice Result

[00114] In the third trial, the objective was to chromatographically separate a sample of Concord grape juice into a Concord grape JCP peak and a sugar peak. The results showed a separation of the Concord grape sample, which contained free ions, pectin, dyes (colors), fructose, glucose, acids, flavor compounds, aroma compounds and other endogenous compounds (contaminants), in a semi-sharp peak of JPC from Concord grape juice and a semi-wide peak of sugar (fructose and glucose). The pH and the addition of ions (cations, anions) were evaluated during the chromatographic separation of Concord grape juice. The other process chromatographic parameters (sample size, flow rate, column diameter and height) of the apple juice were used with the Concord grape juice sample.

[00115] Figure 5 is a graph of the results of a chromatographic separation of Concord grape juice according to exemplary modalities. Referring to Figure 5, Concord grape juice was separated into two chromatographic peaks. The first peak was composed of the Concord grape JCP peak and the second peak was the sugar peak (fructose and glucose). During the process, the original colorant of the Concord grape juice was removed from the flow of Concord grape juice by the resin. The blue dye bound to the resin. Extensive testing was required to determine the ideal pretreatment process for Concord grape juice that would prevent the dye from being removed from the fruit juice stream and binding to the resin. By increasing the pH and adding ions (i.e., calcium chloride) to the sample grape juice, it was possible to significantly reduce the amount of dye that binds to the resin and remains in the Concord grape juice flow.

[00116] The sample of Concord grape juice was separated into two chromatographic peaks. The first peak was composed of the Concord grape JCP peak and the second peak was the sugar peak (fructose and glucose). Although the Concord grape juice sample contained significant amounts of free ions, pectin, glucose, flavors, acids, and other endogenous compounds (contaminants), it was separated into a Concord grape JCP peak and a single broad sugar peak (fructose and glucose), rather than being separated into individual sugar spikes. In addition, the Concord grape JCP peak eluted about 10 ml after the blue colored peak from the first run (dummy juice) due to contaminants present in the Concord grape juice sample. The Concord JCP grape produced a well-defined bell-shaped curve, while the peak sugar (fructose and glucose) produced a positively slanted curve. Tube 4 had the maximum color, acidity and flavor (sensory evaluation), while tubes 8, 9 and 10 had the highest Brix value, as measured with a portable refractometer (Reichert model 10430 0-30 Brix). The assay was conducted in triplicate and showed good reproducibility. The average of the three data sources is shown below in Table 1.

Orange Juice Results

[00117] In the fourth trial, the objective was to chromatographically separate an orange juice sample (without original flavoring oils) into an orange JCP peak and a sugar peak. The orange juice sample was significantly more viscous (thicker) and had a higher concentration of complex mixtures of contaminants than the apple or Concord grape juice samples. The orange juice sample contained free ions, pulp, pectin, fructose, glucose, sucrose, acids, flavor compounds, aroma compounds and other endogenous compounds (contaminants). The results showed a separation of the orange juice sample into an orange JCP peak and a sugar peak (fructose, glucose and sucrose).

[00118] A series of tests was necessary to determine the ideal pretreatment of orange juice. The first sample was from a low pulp orange juice concentrate. The product was diluted with water to 42 Brix and passed through a filter. However, the first orange juice sample clogged the column. The second sample involved using a commercially available pulp-free orange juice concentrate and part of the pectin was removed. The product was diluted in distilled water at 42 Brix and filtered. However, the second orange juice sample also plugged the column. The third sample involved obtaining a commercially available clarified orange juice concentrate. This sample was commercially passed through a membrane filtration system to remove most of the pulp and some of the pectin. The clarified orange juice concentrate was used in the other tests.

[00119] A series of chromatographic parameters were evaluated, which include sample size, flow rate, column height (bed) and pH, together with the clarified samples of orange juice.

[00120] The sample size was evaluated from 10 to 50 ml. The smallest sample size (10 ml) did not exhibit good visual or sensory results for the orange JCP peak. However, it performed better than the apple juice sample. The largest sample size (40 50 ml) clogged the column as the sample was too large, too thick and too viscous. Even raising the column liquid level to raise the column pressure did not solve the problem. Based on the results, it turned out that the optimal sample size is 32 ml.

[00121] Column (bed) heights were evaluated from 40 cm to 100 cm. The shorter column did not produce a good separation of orange JCP peak and sugar peak (fructose, glucose and sucrose). The 100 cm column with the small sample size produced large, broad peaks. The ideal bed height was 63 cm, which produced two separate and distinct peaks.

[00122] Flow rates have been evaluated from 1 to 10 ml/minute. The slower flow rate was too slow and the chromatograms took too long. The fastest flow rates were too fast and distorted the chromatographic peaks. Medium and large sample sizes and tall column obstructed and inhibited flow. Based on the results, it was found that the ideal flow rate is 3.7 ml per minute with the medium column.

[00123] The pH of the orange juice samples was evaluated from a pH of 2 to 6. The pH of the sample affected the separation of the orange juice sample and the chromatographic formats of the orange juice peak and the orange juice peak. sugar.

[00124] Figure 6 is a graph of the results of a chromatographic separation of orange juice according to exemplary modalities. With reference to Figure 6, the orange juice was separated into two chromatographic peaks. The first peak was composed of the orange JCP peak and the second peak was the sugar peak (fructose, glucose and sucrose). Orange juice had the highest concentration of pulp, pectin, orange oils and other contaminants. Orange JPC eluted about 15 ml after the blue peak in the first run and about 5 ml after the apple JCP peak in the second run. Sugar eluted in a single peak rather than individual sugar peaks. The orange JPC produced a well-defined bell-shaped curve, while the sugar peak (fructose, glucose, sucrose) produced a positively slanted curve. Tube 4 had the maximum orange color, orange aroma, acids, orange flavor and other juice components as measured by sensory evaluation (qualitative data), while tube 9 had the highest Brix value as measured with a portable refractometer (Reichert model 10430 0-30 Brix). The assay was conducted in triplicate and showed good reproducibility. The average of the three data sources is shown below in Table 1.

Results of Orange Juice with Chelant

[00125] In the fifth trial, the objective was to chromatographically separate orange juice sample with chelator (eg, EDTA) into an orange juice with peak of JCP and EDTA and a peak of sugar. The results showed a separation of clarified orange juice with EDTA sample into an orange juice with a JCP and EDTA peak and a sugar peak (fructose, glucose and sucrose).

[00126] The same optimal sample size, column height and flow rates of the test orange juice were used for the EDTA orange juice test. The pH of the orange juice with EDTA sample was evaluated from a pH of 2 to 6. The pH of the sample affected the separation and elution of the orange juice with EDTA sample and the chromatographic formats of the orange juice with EDTA peak. JCP and EDTA and the sugar spike.

[00127] Figure 7 is a graph of the results of a chromatographic separation of an orange juice with a chelator, in which the chelator protected the resin complex, according to exemplary embodiments. Referring to Figure 7, the orange juice sample with chelator (eg EDTA) was separated into two chromatographic peaks. The first peak was composed of orange with a peak of JCP and EDTA and the second peak was the peak of sugar (fructose, glucose and sucrose) (Table 1). Orange with JCP and EDTA peak produced a well-defined bell-shaped curve, while sugar peak (fructose, glucose, sucrose) produced a positively oblique curve. Tube 4 displayed the maximum orange color, orange flavor, orange aroma, acids, and other juice components as measured by sensory evaluation (qualitative data). Tube 9 had the highest Brix value as measured with a portable refractometer (Reichert model 10430 0-30 Brix). The assay was conducted in triplicate and showed good reproducibility. Orange juice and orange juice with EDTA showed similar chromatographic and sensory results. The average of the three data sources is shown below in Table 1.

Comparison of Chromatographic Results

[00128] A simulated fruit juice sample containing pure fructose and blue dye was separated into a pure fructose peak and a blue dye peak. The apple juice sample containing free ions, pectin, fructose, glucose, sucrose, acids, flavor compounds, aroma compounds and other endogenous (contaminant) compounds was not separated into clear individual peaks. Contaminants present in the apple juice samples prevented the three sugars from being separated into three individual sugar peaks. Endogenous compounds also affected apple JCP peak elution. The apple JCP peak eluted about 6 ml after the blue colored peak from the first run. Contaminants (free ions, pectin, fructose, glucose, acids, flavor compounds, aroma compounds and other endogenous compounds) present in Concord grape juice prevented the fructose and glucose from splitting into two individual sugar spikes. The sugars eluted as a single broad sugar peak. The Concord grape JCP peak eluted 8 ml after the blue peak in the simulated juice assay. The orange juice sample contained free ions, pulp, pectin, fructose, glucose, sucrose, acids, flavor compounds, aroma compounds and other endogenous compounds (contaminants). The orange juice sample was not separated into three individual sugar peaks (fructose, glucose and sucrose) due to endogenous contaminants. The orange JCP peak from the fourth run and the orange with JCP and EDTA peak from the fifth run eluted about 9 ml after the blue color peak from the first run and about 5 ml after the apple JCP peak from the second run. The results showed that the different composition of the sample (free ions, pulp, pectin, orange oils, fructose, glucose, sucrose, acids, flavor compounds, aroma compounds and other endogenous contaminants) affected the chromatographic separation of the four samples compared with the simulated juice sample. This shows that the compounds present in orange juice had a greater effect on the orange juice chromatography than in the simulated juice, apple juice and Concord grape juice assays. Orange juice not only postponed the peak, but the shape of the peak was also changed. The blue-colored peak was in the shape of a well-defined bell-shaped curve, while the apple JCP, Concord grape JCP, orange JCP, and orange with JCP and EDTA peaks were positively oblique. Sugar peaks (fructose; fructose, glucose and sucrose; or fructose and glucose) produced a positively skewed curve.

EXPERIMENTAL CONCLUSION Mock Juice

[00129] The objective of the first test was to investigate the possibility of separating an aqueous solution with simulated fruit juice containing blue color (no reactivity with the resin), purified fructose and distilled water (free of ions) into an aqueous blue peak and a peak of aqueous fructose with a column of Dowex® Monosphere® 99CA/320 separation resin. The sample introduced was a solution of two pure carbohydrates free of contaminants. The two peaks were purified free of contaminant and free ions. By optimizing sample size, flow rate, column diameter and column height, it was possible to separate the simulated fruit juice into a blue dye solution peak and a sugar (fructose) peak.

fruit juices

[00130] The objective of trials 2-5 was to investigate the possibility of separating a variety of fruit juices, containing different concentrations and composition of peculiar compounds (contaminants) that could interfere with the chromatography of a sample, in a fruit JCP peak and a sugar peak with a Dowex® Monosphere® 99CA/320 separating resin column. The process was able to separate each of the juice samples into a fruit JCP peak and a sugar peak. Fruit juices have different sugar compositions. Furthermore, the characteristics and properties of each resin and the suitable processing parameters are different and therefore need to be investigated.

[00131] The processes discussed here were able to separate solutions and juices with different sugar compositions, which include a simulated juice containing only fructose, a Concord grape juice containing primarily glucose and fructose, and orange and apple juices containing glucose, fructose and glucose.

[00132] Fruit juices contain a wide variety of chemically peculiar compounds and different sugar compositions. Some compounds are known to bind very strongly to calcium (eg pectin); whereas with other compounds, the binding constant with calcium is unknown (eg compounds with an OH hydroxyl group). Some compounds may have very large binding constants, while others may have medium, little, or no interactions with calcium. Calcium forms a weak interaction with the hydroxyl group (OH) on fructose, sucrose and/or glucose molecules. The resin can also interact with hydroxyl groups on other endogenous compounds present in fruit juice. Since the resin complex contains calcium, endogenous compounds could bind calcium, thereby becoming unavailable for chromatography. Endogenous compounds could also have a medium or weak interaction, which would make them interfere with the separation or remain inert with the calcium resin complex. The pre-assay was unknown and it could not be estimated (no reasonable expectation) how the various compounds would affect the chromatographic separation of the different fruit juices.

[00133] Fruit juices contain significant amounts of free ions. Free ions interfere with sample chromatography by dissociating calcium from the calcium resin complex. As the flow of fruit juice continues through the column, the resin becomes less efficient and able to chromatographically separate the fruit juice. The higher the ion concentration in the fruit juice sample, the faster the resin becomes unable to separate the sample. Resin damage is determined by a combination of time (duration) and ion concentration.

Apple juice

[00134] The purpose of the second trial was to investigate the possibility of separating a sample of apple juice concentrate into an apple JCP peak and a sugar peak with a Dowex® Monosphere® 99CA/320 separation resin column. The apple juice sample contained free ions, pulp, pectin, fructose, glucose, sucrose, acids, color, apple flavor compounds and other endogenous compounds (contaminants). The apple juice sample was separated into two peaks. The apple JCP peak contained free ions, apple color (light brown), apple flavor, apple aroma, pectin, acids, and other endogenous contaminants. The sugar peak contained a mixture of three sugars (fructose, glucose and sucrose) and minimal concentrations of pulp, pectin, light brown color, apple flavor, aroma, acids and other endogenous compounds.

[00135] By optimizing the sample size, flow rate, column height and pH, it was possible to separate the apple juice sample into an apple JCP peak and a sugar peak (fructose, glucose and sucrose). The apple JCP peak eluted about 6 ml after the blue color peak in the simulated juice (blue color and fructose solution) from the first run. Results showed that contaminants (eg, free ions, pectin, fructose, glucose, sucrose, acids, flavor compounds, aroma compounds, and other endogenous compounds) interfered with the chromatographic separation of the apple juice sample. The elution and shape of the sugar peak were similar in the simulated juice and apple juice trials.

concord grape juice

[00136] The purpose of the third trial was to investigate the possibility of separating a sample of Concord grape juice into a Concord grape JCP peak and a sugar peak with a column of Dowex® Monosphere® 99CA/320 separation resin. The Concord grape juice sample contained free ions, pulp, pectin, fructose, glucose, dyes, acids, grape flavor compounds and grape aroma compounds and other endogenous compounds (contaminants). Concord grape juice contains fructose, glucose and may contain an identifiable level of sucrose. The Concord grape juice sample was separated into two peaks. The sugar peak contained a mixture of two sugars (fructose and glucose) and minimal concentrations of pulp, pectin, dyes, grape flavor compounds and grape aroma compounds and other endogenous compounds.

[00137] By adjusting the pH and adding free ions (eg, calcium) that bound to the active sites of the dye molecules, it was possible to reduce the amount of dye that is removed from the Concord grape juice sample and absorbed by the resin.

[00138] The Concord grape JCP peak eluted about 8 ml after the blue color peak in the simulated juice assay (blue color and fructose solution). Results showed that contaminants (eg, free ions, pectin, fructose, glucose, acids, flavor compounds, aroma compounds, and other endogenous compounds) interfered with the chromatographic separation of the Concord grape juice sample.

Orange juice

[00139] The purpose of the fourth trial was to investigate the possibility of separating a clarified orange juice sample into an orange JCP peak and a sugar peak with a Dowex® Monosphere® 99CA/320 separation resin column. Most of the pulp and part of the pectin were removed from the sample. Also, some of the orange oils were not added back to the orange juice concentrate. The clarified orange juice had most of its pulp removed and the sample containing free ions, pulp, pectin, orange oils, fructose, glucose, sucrose, orange flavor compounds, orange aroma, acids and other endogenous compounds (contaminants) was separated into an orange JCP peak and a mixed sugars peak. "Orange JPC" fractions contained free ions, orange color, flavor orange, pectin, orange flavor, acids and other endogenous compounds (contaminants). The sugar peak contained a mixture of three sugars (fructose, glucose and sucrose) and minimal concentrations of pulp, pectin, orange color, orange flavor, aroma, acids and other endogenous compounds.

[00140] By optimizing the sample size, flow rate, column height and pH, it was possible to separate the orange JCP peak from the sugar peak (mixed sugars, fructose, glucose and sucrose).

[00141] The orange juice sample contained more pulp, pectin, orange oils and other contaminants than the apple juice sample. The orange juice sample was also significantly thicker and more viscous than the apple juice sample. The orange juice composition affected the chromatographic separation of the sample and delayed the elution of the orange JPC fraction relative to the simulated juice, apple juice, and Concord grape juice samples.

Orange Juice with Quelant

[00142] The aim of the fifth trial was to investigate the possibility of separating a sample of orange juice with a chelator (eg EDTA) into an orange with a peak of JCP and EDTA and a peak of sugar. Orange juice with EDTA sample contained chelated ions, pulp, pectin, orange oils, fructose, glucose, sucrose, orange flavor compounds, orange aroma, acids and other endogenous contaminants. The sample was separated with a Dowex® Monosphere® 99CA/320 separating resin column into two peaks. The "Orange with EDTA and JCP" peak contained orange color, orange flavor, pectin, acids, chelated ions and aroma. The sugar peak contained a mixture of three sugars (fructose, glucose and sucrose) and minimal concentrations of orange color, orange flavor, aroma, acids and other endogenous compounds.

[00143] Using optimization parameters of the assay with clarified orange juice, it was possible to separate the orange with peak JCP and EDTA from the peak sugar (mixed sugars, which includes fructose, glucose and sucrose).

[00144] The chelation of free ions present in the fruit juice sample before introducing the sample into the column proved to be advantageous, since the free ions dissociate calcium from the calcium resin complex, which negatively affects the chromatographic separation of the sample. Free ion chelation protects the calcium resin complex by reducing the ability of free ions to dissociate calcium from the calcium resin complex. Resin granules that are devoid of calcium ions will not be able to separate sugars from juice samples.

[00145] Since the resin complex has a selective attraction for sugars (eg fructose, glucose and sucrose) present in the fruit juice sample, the resulting fruit JCP can be used to produce a low-calorie drink. The drink would not meet standard identification for a "fruit juice", but would meet standard identification for a "fruit juice drink".

[00146] Although processes and products have been described here with reference to various embodiments, those skilled in the art will understand that various changes can be made and that equivalents can be substituted for elements thereof without departing from the scope and essence of the present invention. Furthermore, various modifications can be made to adapt a particular situation or material to the teachings of the present invention without departing from the scope thereof. Therefore, it is intended that the present invention not be limited to the particular embodiments described herein, but rather that it include all embodiments falling within the scope of the appended claims. All citations referenced are expressly incorporated herein by reference.

Claims (33)

A method of producing a low calorie fruit juice beverage, comprising: passing a supply stream of a fruit juice containing endogenous compounds through a bed of resin, the endogenous compounds including sugary juice components and unsweetened, the components of unsweetened juice including original free ions and pectin, the resin having an affinity for sugars; chromatographically separate the fruit juice into concentrated bands of unsweetened juice components and sugars moving through the resin bed, the concentrated band of sugars moving at a slower rate through the resin bed than the concentrated band of unsweetened juice components due to weak attraction between resin and sugars; withdrawing the concentrated band of sugars as a sugar stream from a first extraction point in the resin bed, the sugar stream including at least fructose and glucose, the sugar stream including at least 45% of the sugars in the supply stream and no more than 35% of unsweetened juice components in the supply stream; and withdrawing the concentrated band of unsweetened juice components as a stream of unsweetened juice components from a second extraction point in the resin bed, the second extraction point being downstream of the first extraction point, the sugar-free juice components including a higher concentration of sugar-free juice components than the supply stream or sugar stream, the sugar-free juice component stream containing at least 65% of the sugar-free juice components in the supply stream and no more than 55% of the sugars in the supply stream. Method, according to claim 1, characterized in that the flow of sugar-free juice components includes a greater concentration of endogenous flavor compounds, endogenous aroma compounds, endogenous acids, endogenous minerals and endogenous vitamins than the flow of supply or flow of sugar. Method according to claim 1, characterized in that the method is implemented as a simulated moving bed. Method, according to claim 1, characterized by the fact that the resin bed is arranged in one or more columns. Method according to claim 1, characterized in that the sugar stream includes a higher concentration of fructose, glucose and sucrose or a higher concentration of fructose and glucose than the supply stream or the product stream with sugar components. unsweetened juice according to a weight basis. 🇧🇷 Method according to claim 1, characterized in that the juice components without sugar fraction elute from the resin bed before the sugar flow. Method, according to claim 1, characterized in that the first extraction point is axially positioned so that a peak of the concentrated sugar band is removed from the resin bed with the sugar flow. Method according to claim 1, characterized in that the second extraction point is axially positioned so that a peak of the concentrated band of sugar-free juice components is removed from the resin bed with the flow of juice components no sugar. Method according to claim 1, further comprising: pre-treating the supply stream before passing the supply stream through the resin bed, the pre-treatment including one or more of the steps to reduce or increase the level of a component in the supply stream, dilute the supply stream or concentrate the supply stream. Method, according to claim 1, characterized in that the fruit juice is not subjected to a deionization process before passing through the resin bed. Method, according to claim 1, characterized in that the fruit juice is one or more of: orange juice, tangerine juice, grapefruit juice, grape juice, red wine juice, cranberry juice, juice apple juice, pineapple juice, blackberry juice. Method, according to claim 11, characterized in that the orange juice contains less than 15% by weight (w/w) of pulp. Method according to claim 11, characterized in that the orange juice contains less than 5% by weight (w/w) of pulp. Method according to claim 1, further comprising: adding a chelator to the supply fruit juice stream so that it binds to the original free ions and protects it from a displacement of metal ions in the resin when the flow of fruit juice supply pass through the bed. Method, according to claim 14, characterized by the fact that the chelator forms a bond of ligands with the original free ions. Method according to claim 14, characterized in that the chelating agent is added to the fruit juice in a concentration ranging from 0.0001 to 20%. Method, according to claim 14, characterized in that the chelating agent is added to the fruit juice in a concentration ranging from 0.0001 to 2%. Method according to claim 14, characterized in that the chelator is in the form of an acid or a salt. Method according to claim 14, characterized in that the chelator is at least one of ethylenediaminetetraacetic acid (EDTA) and ascorbic acid. Method, according to claim 1, characterized in that it also comprises: adding ions to the supply flow so that they bind to the active sites of the endogenous compounds of the fruit juice in order to reduce their interaction with the resin. Method according to claim 1, characterized in that it also comprises: concentrating the flow of sugar-free juice components. The method of claim 1, further comprising: adding a sweetener to the stream of unsweetened juice components to produce a low-calorie fruit juice beverage. Method according to claim 22, characterized in that the sweetener is at least one of a high-intensity natural sweetener or a high-intensity artificial sweetener. Method, according to claim 23, characterized by the fact that the high-intensity natural sweetener is stevia. Method, according to claim 23, characterized in that the high-intensity artificial sweetener is at least one of sucralose, aspartame, acesulfame potassium, alitame, cyclamates and saccharin. 🇧🇷 Method according to claim 1, characterized in that the resin is an ion exchange resin containing metal ions that form a weak attraction with the sugars in the fruit juice. Method according to claim 26, characterized in that the resin is a cation exchange resin. Method according to claim 26, characterized by the fact that a linker bond is formed between the resin and the sugars. Method according to claim 26, characterized in that the resin is in salt form. Method according to claim 26, characterized in that the metal ions include at least one of alkali metal ions and alkaline earth metal ions. Method according to claim 30, characterized in that the alkaline earth metal ions are calcium ions. Method according to claim 1, characterized in that the fruit juice is separated into concentrated bands of sugar-free juice components and sugars by means of an exchange chromatography. Method according to claim 1, characterized in that it also comprises: redirecting the remainder of the supply flow from the bottom of the bed to the top of the bed so as to form a recycle flow, the remainder of the flow being a portion from the supply stream that is not part of the sugar stream or the sugar-free juice component stream.

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