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WO-2026090699-A1 - INTEGRATED METHOD USING SOLANUM LYCOCARPUM FRUIT

WO2026090699A1WO 2026090699 A1WO2026090699 A1WO 2026090699A1WO-2026090699-A1

Abstract

The present invention relates to an integrated method using Solanum lycocarpum fruit as a source of raw material, providing a cost-effective method that does not generate toxic residues, requires minimal water input, and preserves the components contained in said fruit from interaction with its pigmented phenolic compounds. The present invention describes, more specifically, a biorefinery method for recovering and reusing the solvents used during the steps thereof, wherein said method comprises six stages aimed at the complete exhaustion of the fruits and the obtainment of six different final products that may be used as precursors or intermediates of new products in various industrial sectors.

Inventors

  • PEREIRA JÚNIOR, Marcos Antonio
  • LIBERATO ALVES, Guilherme

Assignees

  • ALMIR MARTINEZ

Dates

Publication Date
20260507
Application Date
20251029
Priority Date
20241101

Claims (20)

  1. 1. INTEGRATED PROCESS FROM LOBEIRA FRUITS characterized by comprising the following steps: • Stage A comprising: (i) select and sanitize the fruits in a tank (2); (ii) peeling the fruit by mechanical means (3) in the presence of a solution comprising organic acid and/or inorganic acid; wherein at the end of step A are obtained: the peeled fruit and a suspension of peel fragments in acidic solution; • Stage B comprising: (iii) separate the liquid fraction (fl) present in said suspension of shell fragments from the particulate material by means of a separation means (20); (iv) transfer the liquid fraction (fl) to a tank (4) and adjust the hydronium ion concentration so that it is maintained between 2.1 x 10' 6 and 7.9 x 10' 4 mol per gram of fruit; (v) repeat processes (iii) and (iv) until at the end of about 9 to about 15 peeling cycles of step A, said liquid fraction (fl) is sent to a separation medium (5) to obtain the acidic phenolic extract, which then goes to packaging; (vi) direct the solid fraction (fs) obtained in (iii) to the drying medium (6) and packaging; • Stage C comprising: (vii) remove residues from fruit peels by spraying said acidic phenolic extract; (viii) crushing the fruit in a mechanical means (17) in the presence of a solution containing organic acid, inorganic acid and/or combinations thereof; wherein the ratio of peeled fruit to acid is 1:2 (w/v); (ix) transfer the crushed mass to a separation medium (18) and obtain two fractions, said fractions being liquid (Cliq) and solid (Csol); • Stage D comprising: (x) transfer the liquid fraction (Cliq), obtained in (ix), to a centrifuge (19); wherein the supernatant is sent for packaging; wherein said precipitate goes through a sequence of operations alternating washes (7) and centrifugations (8) until neutralization is achieved, wherein the first two wash waters are directed to the treatment of the solid fraction (Csol) in stage E; wherein the remaining waters obtained in the washing process are directed to tank (2) of stage A; wherein said precipitate is sent to an air dryer (9) until it reaches a moisture content of less than 13% for subsequent packaging; • Stage E, including: (xi) homogenize in a reactor (10) the solid fraction (Csol), obtained in (ix), with the wash water obtained in step D; wherein the proportion of Csol to wash water is 1:3 to 1:50 (w/v); (xii) adjust the reaction mixture so that the hydronium ion concentration is maintained between 2.0 x10' 6 and 2.0 x10 -4 mol per gram of Csol, by adding a solution comprising organic acid, inorganic acid and/or combinations thereof; (xiii) heat the reaction mixture between 40 °C and 95 °C for 30 to 90 minutes; (xiv) separate the reaction mixture obtained in said step E in a separation medium (15); (xv) obtaining a supernatant (Eliq) and a precipitate (Eppt); wherein said precipitate (Eppt) is dried under an air stream (11) and subsequently packaged; wherein said supernatant (Eliq) is sent to a cooling tank (12); • Stage F comprising: (xvi) cool the supernatant (Eliq); (xvii) react the supernatant (Eliq) with C2-5 alcohol; (xviii) separate the reaction material in a separation medium (16), obtaining a particulate material in the reaction medium (Fpmr) and a liquid fraction; (xix) drying in a medium under air flow (13) said particulate material in the reaction medium (Fpmr); (xx) distill the remaining liquid in the reactor into a medium (14), in which the C2-5 alcohol is recovered and redirected to the tank (12).
  2. 2. PROCESS, according to claim 1, characterized in that the fruits are of the species Solanum lycocarpum, or Solanum crinitum, or Solanum grandiflorum.
  3. 3. PROCESS, according to any one of claims 1 to 2, characterized in that step A comprises a platform coupled to a perforated conveyor belt (1) for sorting the fruit.
  4. 4. PROCESS, according to any one of claims 1 to 3, characterized in that the sanitization step further comprises the addition of a chemical agent, a physical agent or combinations thereof, wherein the chemical agent is selected from the group consisting of ozone gas, chlorine gas, sodium hypochlorite, hydrogen peroxide, acetic acid, peracetic acid, hydrochloric acid, perchloric acid, hypochlorous acid; wherein the physical agent is selected from the group consisting of ozonation, electrolysis with or without bubbling of chlorine gas, UV-C radiation (180-280 nm), UV radiation (4-400 nm) or gamma radiation.
  5. 5. PROCESS, according to any one of claims 1 to 4, characterized in that the concentration of the chemical agent varies from 0.2% to 70% by volume per gram of fruit.
  6. 6. PROCESS, according to any one of claims 1 to 5, characterized in that the chemical agent is ozone gas at a flow rate of 300 L/h to 2000 L/h for 30 to 240 min, preferably at a flow rate of 900 L/h for 90 min.
  7. 7. PROCESS, according to any one of claims 1 to 6, characterized in that the tank (2) employed in step A is a washing tank with swirl agitation.
  8. 8. PROCESS, according to any one of claims 1 to 7, characterized in that the organic acid used in steps A, B and E is selected from the group consisting of lactic acid, pyruvic acid, acetic acid, oxalic acid, citric acid, aconitic acid, succinic acid, fumaric acid, malic acid, malonic acid, ascorbic acid, erythorbic acid, phthalic acid, salicylic acid, acetylsalicylic acid, benzoic acid, cinnamic acid, ferulic acid, coumaric acid, gallic acid, pelagic acid, or their derivatives, preferably selected from cinnamic acid, citric acid, acetic acid, ascorbic acid or lactic acid.
  9. 9. PROCESS, according to any one of claims 1 to 8, characterized in that the inorganic acid used in steps A, B and E is selected from the group consisting of chloric acid, hydrochloric acid, acid Chlorous acid, hypochlorous acid, perchloric acid, phosphoric acid, phosphorous acid, polyphosphoric acid, pyrophosphoric acid, nitric acid, nitrous acid, mixtures thereof or mixtures with their sodium salt derivatives or their potassium salt derivatives, preferably selected from phosphoric acid or nitric acid.
  10. 10. PROCEDURE, in accordance with any of the claims. I a 9, characterized in that the concentration of organic acid in step A is from 0.0040% to 0.020% mol, preferably 0.0042% to 0.013% mol; and the concentration of inorganic acid in step A is from 0.005% to 0.5% mol, preferably 0.005% to 0.01% mol.
  11. 11. PROCESS, according to any one of claims 1 to 11, characterized in that, in processing (ii) of step A and in step C, the hydronium ion concentration is maintained in the range of 2.1 x 10' 6 to 1.6 x 10' 3 mol of hydronium ions per gram of fruit.
  12. 12. PROCESS, according to claim 11, characterized in that the concentration of organic acid is maintained at a minimum of 8.3 x 10⁻⁵ mol per gram of fruit.
  13. 13. PROCESS, according to any one of claims 1 to 12, characterized in that the solid fraction (fs) obtained in step B comprises the fruit peels.
  14. 14. PROCESS, according to any one of claims 1 to 2, characterized in that said fruits have a diameter in the range of 4 to II centimeters, preferably 6 to 11 cm, preferably 8 cm.
  15. 15. PROCESS, according to claim 1, characterized in that the mechanical means (3) of step A is a peeler.
  16. 16. PROCESS, according to any one of claims 1 to 15, characterized in that in step A, the fruits are held in the mechanical medium (3) for a time sufficient to remove at least 80% of the peel covering, preferably 90% of the peel covering.
  17. 17. PROCESS, according to any one of claims 1 to 16, characterized in that in steps B, C, E and F, the separation means (20, 5, 18, 15, 16) is a centrifuge, decanter, filter or combinations thereof.
  18. 18. PROCESS, according to any one of claims 1 to 17, characterized in that in step B, the drying medium (6) is an airflow dryer.
  19. 19. PROCESS, according to any one of claims 1 to 18, characterized in that in (viii) in step C, the temperature is between 10 °C and 50 °C, preferably between 10 °C and 20 °C; wherein the browning content is below 10%.
  20. 20. PROCESS, according to any one of claims 1 to 19, characterized in that in (x) in step D, the drying temperature in the air dryer (9) is in the range of 25 °C to 50 °C, preferably between 30 °C and 40 °C.

Description

INTEGRATED PROCESS FROM WOLF FRUITS FIELD OF THE INVENTION The present invention relates to an integrated process using lobeira fruit as a raw material source. More specifically, the present invention relates to processing leading to the complete exhaustion of the raw material and the obtaining of six different end products, with the reuse of solvents throughout said process and without the generation of toxic waste. BACKGROUND OF THE INVENTION The lobeira, popularly known as jurubebão, juripeba, jurepeba, baba-de-boi, fruta-do-lobo or guarambá, is a plant species found in devastated areas, primary scrubland, secondary formations in high places and along roadsides throughout Brazil, more specifically in the states of Amazonas, Goiás, Maranhão, Mato Grosso, Mato Grosso do Sul, Minas Gerais, Pará, Paraná, Rio de Janeiro, São Paulo and Tocantins. Because it is a hardy plant tolerant of unfavorable environmental conditions, it is considered by ranchers to be a pasture pest, as it grows in different types of soil, such as sandy soils, poor in nutrients, acidic soils, with a pH between 4.5 and 5.5. Furthermore, the lobeira plant is characterized by its resistance to temperatures ranging from -2°C (during frosts) to 40°C (in arid climates), fire resistance, and its ability to withstand seasonal water stress. For example, the lobeira does not require much soil moisture, growing well with a minimum of 600 to 1,200 millimeters of annual rainfall. As for fruiting, this begins between 2 and 3 years after planting, and the fruits can weigh up to 1.3 kg. Due to its diverse components, the lobeira plant has been studied primarily for use in the food industry, for example, as a source of starch, and in the pharmaceutical industry. However, there is very little information related to the extraction of its major components, as well as its large-scale processing. Currently, it is observed that the studies being developed are limited to obtaining a single component or a fraction of components from the fruits of the lobeira plant, employing isolated methods for the individual extraction of each component. Patent No. PI1000753-9 discloses an extraction process for obtaining starch from wolf apple (Solatium lycocarpum St. Hil), in which The selected fruits were washed, peeled, and chopped; the seeds were removed; the pulp was crushed; and the resulting starch was filtered, decanted, washed twice with distilled water, and dried in a forced-air oven. However, after successive washing and decantation steps, two fractions are obtained (one clear and one dark at the bottom of the flask), resulting in a low-quality starch since it is contaminated with adsorbed pigmented phenolic compounds. Furthermore, the yield is low, on the order of 2.6% on a wet basis. Patent application no. PI 0305446-2 aims to provide a water-soluble extract obtained from a plant of the genus Solanum to be used as an active component in a pharmaceutical composition, consisting essentially of at least 60% to 90% solamargine and solasonine, and which can be directly dissolved in pure water with a neutral pH value without the addition of any other solvent and/or solvent adjuvant, thus forming a clear and transparent yellowish aqueous solution with a water solubility ranging from 2 to 20 mg/mL or more. However, it is noted that such processing is not feasible for the lobeira plant, as it would imply grinding an entire plant, according to the preferred embodiment of said application. Furthermore, said patent application aims to obtain the alkaloids solamargine and solasonine, which is not the intention of the present invention. Pascoal, A. M. et al. (“Extraction and chemical characterization of starch from S. lycocarpum fruits”, Carbohydrate Polymers 98 (2013), pp. 1304-1310) report a process for the extraction and chemical characterization of starch from S. lycocarpum fruits, in which citric acid was used as an inhibitor of enzymatic browning. However, citric acid is among the least effective inhibitors for inhibiting enzymatic browning, since its action is notably as an antioxidant agent and not as an inhibitor of the polyphenol oxidase enzyme present in the pulp of lobeira fruits, having an efficacy of 24.3%. Furthermore, this efficacy is dependent on the concentration of polyphenol oxidase, which is intrinsically related to the stage of fruit maturation. Thus, the extraction process used will be effective for a very restricted range of fruits, leading to a limitation of the processing methodology on an industrial scale. Additionally, sodium hydroxide is used to neutralize citric acid and ethanol, generating a highly corrosive residue that requires treatment for its disposal. Já Mota, RDP et al. (“Elaboration and Characterization of Films”) The scientific journal of the SENAI Roberto Mange Faculty of Technology (Jan/Jun 2009), pp. 44-50 - ISSN 1981-8521, reports the extraction of starch from the grinding of the pulp of wolfberry fruits in the presence of a sodium