EP2967093A1 - Revêtements comestibles de nano-cellulose et leurs utilisations - Google Patents

Revêtements comestibles de nano-cellulose et leurs utilisations

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Publication number
EP2967093A1
EP2967093A1 EP14769964.9A EP14769964A EP2967093A1 EP 2967093 A1 EP2967093 A1 EP 2967093A1 EP 14769964 A EP14769964 A EP 14769964A EP 2967093 A1 EP2967093 A1 EP 2967093A1
Authority
EP
European Patent Office
Prior art keywords
composition
plant
fruit
cellulose
coated
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP14769964.9A
Other languages
German (de)
English (en)
Inventor
Yanyun Zhao
John Simonsen
George CAVENDER
Jooyeoun JUNG
Leslie H. Fuchigami
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Oregon State University
Original Assignee
Oregon State University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Oregon State University filed Critical Oregon State University
Publication of EP2967093A1 publication Critical patent/EP2967093A1/fr
Withdrawn legal-status Critical Current

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Classifications

    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23B—PRESERVING, e.g. BY CANNING, MEAT, FISH, EGGS, FRUIT, VEGETABLES, EDIBLE SEEDS; CHEMICAL RIPENING OF FRUIT OR VEGETABLES; THE PRESERVED, RIPENED, OR CANNED PRODUCTS
    • A23B7/00—Preservation or chemical ripening of fruit or vegetables
    • A23B7/16—Coating with a protective layer; Compositions or apparatus therefor
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/005—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by heating using irradiation or electric treatment
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D101/00—Coating compositions based on cellulose, modified cellulose, or cellulose derivatives
    • C09D101/02—Cellulose; Modified cellulose
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs

Definitions

  • This disclosure relates to the field of protective coatings, particularly coatings for plants, plant parts, and foodstuffs. It further relates to compositions for forming protective films and methods of making and using these compositions and coatings.
  • Coatings should be edible and once applied, act as a barrier to moisture, gases and/or UV light, and undesirable microorganisms. However, several other criteria are also important: the coating should be essentially harmless to consumers, transparent (or nearly so) in the visible region so the coated product is visible to the consumer, and it should impart no significant odor or taste to the foods.
  • Anthocyanins provide the majority of red, purple, and blue pigmentation of some fruits and vegetables, and their greater consumption has been suggested to mitigate the risk of chronic disease in humans.
  • these pigments are highly labile and vulnerable to degradation during thermal processing. Further complicating matters is their water- solubility that promotes their leaching into aqueous media.
  • innovative technologies are needed to overcome long- standing technical barriers experienced by the food industry to retain these health-promoting pigments during food handling and processing.
  • Exposure to high levels of UV light can damage developing and maturing produce creating visibly damaged and discolored tissues, destroying native healthful phytochemical compounds, stimulating production of undesirable and harmful compounds like ethylene gas, and providing a foothold for spoilage organisms to grow.
  • Such produce suffers a loss of perceived quality, reduced health benefits and is generally deemed unsuitable for the fresh market. Further, the phenomenon can potentially ruin a grower economically, as the conditions leading to its occurrence are shared by the entire crop.
  • Fresh produce damage can be caused by both external and internal influences. External influence is the most common and can be easily seen when fresh produce cracks in the rain.
  • Drip loss Previously frozen foods typically exude liquid during thawing, resulting in a phenomenon called "drip loss.” This can be off-putting to consumers, and can change the overall composition of the thawed product, making it behave differently from fresh during preparation/cooking. Drip loss also can cause economic losses to the processors.
  • the innovations described herein utilize a cellulose nanomaterial, which has not previously been used as or in edible coatings, alone or in combination with nano calcium carbonate and/or other additives.
  • the resultant coatings are useful for the protection against moisture loss and UV damage of fresh fruits and vegetables both pre- and post-harvest, as a barrier coating for fresh and processed foods, for reducing or preventing leaching of food substances, such as anthocyanins and other water soluble compounds, as well as loss and/or gain of moisture and gases (e.g. , 0 2 and C0 2 ) during food processing and storage.
  • Coatings provided herein are also useful to protect against and reduce biotic and abiotic stresses in plants, plant parts, and foodstuffs while in storage, on the shelf, and during production (including post-harvest production).
  • the composition is a nanocellulose-based edible composition selected from one or more components that form a barrier to biotic and abiotic stresses, water resistant film forming matrices, UV protectants, preservatives (such as foodstuff preservatives), and anti-leaching solutions, wherein the components form a protective barrier when placed on an inorganic material, a foodstuff, a plant or any part thereof, an animal tissue, or any other organic material.
  • compositions comprising a cellulose nanomaterial in an amount ranging from about 0.1 wt/v to about 10 wt/v , an inorganic salt component in an amount ranging from about 0.005 wt/v to about 2.5 wt/v , and a crosslinking agent in an amount ranging from about 0.05 wt/v to about 0.1 wt/v .
  • the composition comprises a cellulose nanomaterial in an amount ranging from about 0.1 wt/v to about 10 wt/v , and an inorganic salt component in an amount ranging from about 0.005 wt/v to about 5 wt/v .
  • the composition comprises a cellulose nanomaterial and at least one additional component selected from a stabilizing agent, an additive agent, an agricultural agent, and combinations thereof.
  • Plants or plant parts comprising a film formed from a composition disclosed herein also are disclosed.
  • embodiments of the disclosed methods comprise substantially coating a plant or plant part with an embodiment of the composition disclosed herein before or after the plant or plant part is harvested or planted.
  • Some disclosed embodiments concern a nano-cellulose edible coating essentially as described herein.
  • a method of coating an object comprising applying to the object a nanocellulose coating or coating composition essentially as described herein also is disclosed.
  • FIGS. 1A and IB are schematic diagrams illustrating the features of an embodiment of the disclosed coating composition (FIG. 1A) that can be used in combination with processing composition embodiments to promote anthocyanin retention in fruits during thermal processing (FIG. IB).
  • FIG. 2 is a schematic diagram illustrating various embodiments of the thermal processing method steps disclosed herein.
  • FIGS. 3A-3E are photographic images of coated and uncoated blueberries after performing two thermal processing steps, film removal, and storage in packing water (one day under ambient conditions).
  • FIG. 3A is an image of uncoated blueberries
  • FIG. 3B is an image of blueberries that were coated with a composition comprising 1% cellulose nanofibrils (CNF) prior to the first thermal processing step
  • FIG. 3C is an image of blueberries coated with a composition (prior to drying) comprising 1% cellulose nanofibrils and 0.01% nano calcium carbonate (NCC) prior to the first thermal processing step
  • FIG. 3D is an image of blueberries coated with a composition comprising 1% cellulose nanofibrils applied by spray coating prior to the first thermal processing step
  • FIG. 3E is an image of blueberries coated with a composition comprising 1% cellulose nanofibrils and 0.01% NCC applied by spray coating prior to the first thermal processing step.
  • FIGS. 4A-4C are photographic images of blueberries coated with different composition embodiments disclosed herein after different thermal processes.
  • FIG. 4A is an image of blueberries after thermal processing at 80 °C for 20 minutes, with the blueberries being coated with CNF prior to thermal processing;
  • FIG. 4B is an image of the blueberries illustrated in FIG. 4A after the coating was removed and the blueberries were subjected to another thermal process at 65 °C for 15 minutes;
  • FIG. 4C is an image of the blueberries of FIGS. 4A and 4B after being stored in water for one day under ambient conditions.
  • FIG. 5 is a graph of monomeric anthocyanin concentration (mg/L) and pigment absorbance (measured at 525 nm) leached from coated or uncoated blueberries after processing (80 °C for 20 minutes) and cooling (20 minutes).
  • FIG. 6 is a graph of monomeric anthocyanin concentration (mg/L) and pigment absorbance (measured at 525 nm) leached from processed blueberries (first at 80 °C for 20 minutes and then at 65 °C for 15 minutes) after storage (one day, under ambient conditions).
  • FIGS. 7A-7F are photographic images of blueberries after being subjected to thermal processing at 80 °C for 20 minutes and cooling at room temperature for 4 hours.
  • FIGS. 7A-7C are images of a control sample (uncoated blueberries) after 1 hour, 2 hours, and 4 hours, respectively.
  • FIGS. 7D-7F are images of blueberries coated with a composition comprising 1.5% cellulose nanofibrils and 1.0% CaCl 2 after 1 hour, 2 hours, and 4 hours, respectively.
  • FIG. 8 is a bar graph of absorbance (measured at 525 nm) measured from the samples illustrated in FIGS. 7A-7F.
  • the bar graph illustrates changes in the color of the filling solution after the blueberries were subjected to thermal processing at 80 °C for 20 minutes, followed by cooling at room temperature for 4 hours; the results after 1 hour, 2 hours, and 4 hours are presented left to right.
  • "NF1.5CC” indicates the samples coated with a composition comprising 1.5% cellulose nanofibrils and 1.0% CaCl 2 .
  • FIGS. 9A and 9B are photographic images illustrating how embodiments of the disclosed composition can reduce or eliminate leaching of anthocyanin pigments from cherries.
  • FIG. 9A is an image of uncoated cherries
  • FIG. 9B is an image of cherries coated with a composition comprising 1.5% cellulose nanofibrils and 1.0% CaCl 2 .
  • FIGS. 10A and 10B are photographic images illustrating the appearance of uncoated and coated apple rings after freezing processes.
  • FIG. 10A illustrates uncoated apples and
  • FIG. 10B is an image of apple rings coated with a composition comprising 1% cellulose nanofibrils and 0.01% NCC.
  • FIG. 11 is a graph of tensile strength (MPa, N/mm ) and elongation at break (%) illustrating results obtained from analyzing films of carboxymethyl cellulose and films made using various embodiments of the disclosed composition.
  • the different letters provided on the bars in FIG. 11 represent significant difference (P ⁇ 0.05) of tensile strength; where the same letter is indicated, no significant difference was observed.
  • FIGS. 14A-14E are photographic images of treated apples after UV exposure and storage.
  • FIG. 14A is an image of uncoated apples
  • FIG. 14B is an image of an apple coated with a composition comprising 1% cellulose nanofibrils
  • FIG. 14C is an image of an apple coated with a composition comprising 1% cellulose nanofibrils and 0.01% NCC
  • FIG. 14D is an image of an apple coated with a composition comprising 1% cellulose nanofibrils , applied by spray coating
  • FIG. 14E is an image of an apple coated with a composition comprising 1% cellulose nanofibrils and 0.01% NCC, applied by spray coating.
  • FIGS. 15A-15D are photographic images of uncoated pears after being stored under ambient conditions for 10 days (FIG. 15A) and 25 days (FIG. 15C); pears coated with a composition comprising 1.5% cellulose nanofibrils and 0.1% CaCl 2 stored in the same ambient conditions for 10 days (FIG. 15B) and 25 days (FIG. 15D) also are illustrated.
  • FIGS. 16A and 16B are photographic images of uncoated apples that were stored for 25 days under ambient conditions (FIG. 16A) and apples coated with a composition comprising 1.5% cellulose nanofibrils and 0.1% CaCl 2 that also were stored for 25 days under ambient conditions (FIG. 16B).
  • FIGS. 17A-17D are photographic images of uncoated cherries (FIG. 17A); cherries coated with a composition comprising 2% cellulose nanofibrils (FIG. 17B); cherries coated twice with a composition comprising 2% cellulose nanofibrils (FIG. 17C); and cherries coated with a composition comprising 2% cellulose nanofibrils and 2% CaC0 3 (FIG. 17D).
  • FIG. 18 is a graph of weight gain of cherries (%) and weight loss of water from a container (%) in which the cherries illustrated in FIGS. 17A-17D were soaked for 8 hours.
  • FIGS. 19A-19E are photographic images of cherries coated with 1.5% cellulose nanofibrils and different concentrations of CaC0 3 .
  • FIG. 19A is an image of cherries coated with 1.5% cellulose nanofibrils and 0.01% CaC0 3 ;
  • FIG. 19B is an image of cherries coated with 1.5% cellulose nanofibrils and 0.05% CaC0 3 ;
  • FIG. 19C is an image of cherries coated with 1.5% cellulose nanofibrils and 0.1% CaC0 3 ;
  • FIG. 19D is an image of cherries coated with 1.5% cellulose nanofibrils and 0.5% CaC0 3 ;
  • FIG. 19E is an image of cherries coated with 1.5% cellulose nanofibrils and 1% CaC0 3 .
  • FIGS. 20A-20E are photographic images of cherries coated with 1.5% cellulose nanofibrils and different concentrations of wollastonite (FIG. 20A, 0.17% wollastonite; FIG. 20B, 0.38% wollastonite; FIG. 20C, 0.64% wollastonite; FIG. 20D, 1% wollastonite; and FIG. 20E, 1.5% wollastonite).
  • FIG. 21A 1.5% cellulose nanofibrils and 0.17% nano calcium silicate
  • FIG. 21B 1.5% cellulose nanofibrils and 0.38% nano calcium silicate
  • FIG. 21C 1.5% cellulose nanofibrils and 0.64% nano calcium silicate
  • FIG. 21D 1.5% cellulose nanofibrils and 1% nano calcium silicate
  • FIG. 21E 1.5% cellulose nanofibrils and 1.5% nano calcium silicate).
  • FIGS. 22A-22E are photographic images of cherries coated with 1.5% cellulose nanofibrils added with different concentrations of micro CaC0 3 or CaCl 2 .
  • FIG. 22A uncoated cherries
  • FIG. 22B 1.5% cellulose nanofibrils and 0.1% CaC0 3
  • FIG. 22C 1.5% cellulose nanofibrils and 0.5% CaC0 3
  • FIG. 22D 1.5% cellulose nanofibrils and 0.1% CaCl 2
  • FIG. 22E 1.5% cellulose nanofibrils and 0.5% CaCl 2 ).
  • FIGS. 23A-23H are photographic images of blueberries coated with compositions of 1% cellulose nanofibrils (CNF) comprising different concetrations of carboxymethyl cellulose (CMC), nano calcium carbonate (NCC) , and CaCl 2 .
  • CNF carboxymethyl cellulose
  • NCC nano calcium carbonate
  • CaCl 2 a carboxymethyl cellulose
  • FIGS. 23A-23H are photographic images of blueberries coated with compositions of 1% cellulose nanofibrils (CNF) comprising different concetrations of carboxymethyl cellulose (CMC), nano calcium carbonate (NCC) , and CaCl 2 .
  • SA sodium alginate
  • FIG. 23 A 1% CNF composition further comprising 0% CMC, 0.1% NCC , and 0% CaCl 2
  • FIG. 23B 1% CNF composition further comprising 0.1% CMC, 0.1% NCC, and 0% CaCl 2
  • FIG. 23C 1 % CNF composition further comprising 0% CMC, 0.1% NCC, and 0.1 % CaCl 2
  • FIG. 23D 1 % CNF composition further comprising 0.1% CMC, 0.1% NCC, and 0.1% CaCl 2 (washed off and subjected to a second thermal process at 85 °C for 20 min)
  • FIG. 23E 1% CNF composition further comprising 0% CMC, 0.5% NCC, and 0% CaCl 2
  • FIG. 23F 1% CNF composition further comprising 0.1% CMC, 0.5% NCC , and 0% CaCl 2
  • FIG. 23G 1% CNF composition further comprising 0% CMC, 0.5% NCC, and 0.1% CaCl 2
  • FIG. 23H 0.1% CMC, 0.5% NCC, and 0.1% CaCl 2 ).
  • FIGS. 24A-24H are photographic images of lueberries coated with compositions
  • FIG. 24A is an image of a control batch of blueberries that were not coated;
  • FIG. 24B illustrates blueberries coated with a composition comprising 0.5% CNF and 0.1% CMC, and further comprising 0.1% NCC and 0% CaCl 2 ;
  • FIG. 24C illustrates blueberries coated with a composition comprising 0.5% CNF and 0.1% CMC, and further comprising 0.1% NCC and 0.1% CaCl 2 ;
  • FIG. 24A is an image of a control batch of blueberries that were not coated;
  • FIG. 24B illustrates blueberries coated with a composition comprising 0.5% CNF and 0.1% CMC, and further comprising 0.1% NCC and 0% CaCl 2 ;
  • FIG. 24C illustrates blueberries coated with a composition comprising 0.5% CNF and 0.1% CMC, and further comprising 0.1% NCC and 0.1% CaCl 2 ;
  • FIG. 24D illustrates blueberries coated with a composition comprising 0.5% CNF and 0.1% CMC, and further comprising 0.5% NCC and 0% CaCl 2
  • FIG. 24E illustrates blueberries coated with a composition comprising 0.75% CNF and 0.1% CMC, and further comprising 0.1% NCC and 0% CaCl 2
  • FIG. 24F illustrates blueberries coated with a composition comprising 0.75% CNF and 0.1% CMC, and further comprising 0.1% NCC and 0.1% CaCl 2
  • FIG. 24G illustrates blueberries coated with a composition comprising 0.75% CNF and 0.1% CMC, and further comprising 0.5% NCC and 0% CaCl 2 (washed off and applied the second thermal process at 85 °C for 20 min)
  • FIG. 24H illustrates blueberries coated with a composition comprising 0.75% CNF and 0.1% CMC, and further comprising 0.5% NCC and 0.1% CaCl 2 .
  • FIGS. 25A-25E are photographic images of blueberries coated with compositions comprising various different amounts of CNF, carboxymethyl cellulose, and nano calcium carbonate (CaC0 3 ) and further having been exposed (after being coated) to an aqueous solution of 0.25% sodium algiate (SA) and 18% sugar and two thermal processing steps.
  • FIG. 25A is an image of a control sample where no coating was applied before thermal processing.
  • FIG. 25B illustrates blueberries coated with a composition comprising 1 % CNF/0.1% CMC/0.1% NCC after thermal processing;
  • FIG. 25C illustrates blueberries coated with a composition comprising 1% CNF/0.1% CMC/0.5% NCC after thermal processing;
  • FIG. 25D illustrates blueberries coated with a composition comprising 0.5% CNF/0.1% CMC/0.1% NCC after thermal processing
  • FIG. 25E illustrates blueberries coated with a composition comprising 0.75% CNF/0.1% CMC/0.5% NCC after thermal processing.
  • FIG. 26 is a graph of monomeric anthocyanin concentration (mg/L) and pigment absorbance (measured at 525 nm) leached from the coated or uncoated blueberries illustrated in FIGS. 25A-25E after processing using the 0.25% sodium alginate and 18% sugar processing composition and two steps of thermal processing at 91-93 °C for 9-10 minutes.
  • Treatment I 1% CNF/0.1% CMC/0.1% NCC
  • Treatment II 1% CNF/0.1% CMC/0.5% NCC
  • Treatment III 0.5% CNF/0.1% CMC/0.1% NCC
  • Treatment IV Treatment 0.75% CNF/0.1% CMC/0.5% NCC.
  • FIG. 27 is a graph illustrating changes of monomeric anthocyanin pigment in the blueberries illustrated in FIGS. 26A-26E after being subjected to the second thermal process step; data are reported as the % change in comparison with the first thermal process at 91-93 °C for 9-10 minutes; and the bars of the graph represent the % increase in unstable monomeric anthocyanin pigments, whereas the curve represents the percent polymeric color of the fruit.
  • Treatments I- IV are as indicated in FIG. 26.
  • FIGS. 28A-28C are photographic images of the aqueous solution obtained after thermal processing of a control sample (FIG. 28A) after two thermal processing steps, and a sample wherein the fruit was coated with a composition comprising 1% celluose nanofibrils (CNF)/0.1% carboxymethyl (CMC)/0.5% nano calcium carbonate (NCC) and subjected to a first thermal processing step (FIG. 28B) and then a second thermal processing step (FIG. 28C).
  • CNF celluose nanofibrils
  • CMC carboxymethyl
  • NCC nano calcium carbonate
  • FIGS. 29A-29E are photographic images of blueberries coated with a composition comprising 1% CNF/0.1% CMC/0.5% NCC, wherein the blueberries are added to a processing solution comprising 0.25% carboxymethyl cellulose (CMC) and 18% sugar at various pH values.
  • FIG. 29A is an image of the blueberries in the processing solution after a first and second thermal process step using 0.25% CMC/18% sugar
  • FIG. 29B is an image of the blueberries in the processing solution after a first and second thermal process step using 0.25% CMC/18% sugar and after having been stored for 7 days;
  • 29C is an image of the blueberries in the processing solution after a first thermal processing step using 0.25% CMC/18% sugar and second thermal processing step using 0.25% CMC/18% sugar/10 mM CaCl 2
  • FIG. 29D is an image of the blueberries in the processing solution after a first thermal processing step using 0.25% CMC/18% sugar and second thermal processing step using 0.25% CMC/18% sugar/10 mM CaCl 2 and after being stored for 7 days
  • FIG. 29E is an image of the blueberries in the processing solution after a first processing step using 0.25% CMC/18% sugar and second thermal process using 0.25%
  • FIG. 30 is a graph of monomeric anthocyanin pigment concentration (mg/L) of the various different blueberry embodiments described in FIGS. 29A-29E.
  • FIG. 31 is an image of uncoated blueberries that have undergone high hydrostatic pressure treatment.
  • FIG. 32 is an image of mixed fruit samples that may be coated with the coating compositions disclosed herein.
  • FIG. 33 is a graph illustrating the weight loss of uncoated and coated fruits (the coated fruits coated with a composition comprising 1.5% CNF and 0.1% NCC applied by spraying) during 14 days of storage.
  • FIGS. 34A-34F is a series of photographic images of uncoated and coated mangoes after 14 days of storage at the ambient conditions.
  • FIGS. 34A and 34B uncoated mangoes
  • FIGS. 34C and 35D Coating A, which contains 1.5% cellulose nanofibrils (CNF)/0.1% nano calcium carbonate (NCC) applied by spray method
  • FIGS. 34E and 34F Coating B, which contains 1.5% CNF/0.1% NCC/0.1% carboxymethyl cellulose (CMC) applied by spray method.
  • CNF cellulose nanofibrils
  • NCC nano calcium carbonate
  • FIGS. 34E and 34F Coating B, which contains 1.5% CNF/0.1% NCC/0.1% carboxymethyl cellulose (CMC) applied by spray method.
  • CMC carboxymethyl cellulose
  • Photographs of coated mangoes were taken after film was removed using tap water.
  • FIG. 35 is a graph of the firmness (expressed in Newtons, "N") of the mangoes illustrated in FIGS. 34A-34F.
  • FIGS. 36A-36C are photographic images of grapes illustrating the effect of cinnamon leaf essential (CLE) oil on cellulose nanofibrils (CNF)/nano calcium carbonate (NCC) coating composition.
  • FIG. 36A illustrates uncoated grapes;
  • FIG. 36B CNF/NCC with 2.5% CLE;
  • FIG. 36C CNF/NCC/carboxymethyl cellulose (CMC) with 2.5% CLE.
  • FIG. 37 is a graph illustrating weight loss of uncoated and coated papayas after 3 days of storage under ambient conditions, and exemplary citrus fruits after 5 days during storage under ambient conditions.
  • A refers to a coating composition comprising 1.5% cellulose nanofibrils (CNF)/0.1% nano calcium carbonate (NCC) with 2.5% cinnamon leaf essetial oils (CLE);
  • B refers to a coating composition of CNF/NCC/carboxymethyl cellulose (CMC) with 2.5% CLE.
  • compositions comprising at least one cellulose nanomaterial and an inorganic salt component.
  • the disclosed compositions are useful for forming edible coatings/films on plants, plant parts, and other objects.
  • the compositions further comprise a crosslinking agent.
  • the disclosed compositions and coatings/films made using the compositions are effective at protecting fresh and processed produce and other substances and products, from various different types of food processing damage (and the deleterious effects associated therewith), and biotic and/or abiotic stresses that reduce quality and marketability.
  • Disclosed embodiments include a coating composition useful for preventing pre- and post- harvest damage to plants or parts thereof.
  • the coating compositions mitigate the leaching of inorganic materials, plant and animal tissue pigments, and nutrients in fresh and processed tissues (e.g. , fruits and vegetables).
  • Embodiments of the composition can be used to form a film on objects, such as plants and/or plant parts (e.g. , fruits, vegetables, and the like).
  • compositions, and films made using the composition can function to protect the plant and/or plant part from damage caused by pre- or post-harvest damage and/or processing.
  • agricultural crop seeds and plantlets can benefit from the compositions described herein as they can be protected against biotic and abiotic stresses while in storage and during field production.
  • the disclosed composition, and films made using the composition can prevent reduced perceived quality and reduced health benefits associated with plants or plant parts that have been exposed to, and damaged by, UV light.
  • the compositions, and films made using the compositions can protect foodstuffs, fruits, or vegetables that are stored cold (e.g. , that are frozen, stored in cold rooms or refrigerators). For example, previously frozen foods typically exhibit "drip loss," which can be reduced using the compositions described herein.
  • Embodiments of the composition also can be used to prolong the integrity and appearance of foodstuffs and fresh produce.
  • Some embodiments concern a composition, comprising a cellulose nanomaterial in an amount ranging from about 0.1 wt/v to about 10 wt/v ; an inorganic salt component in an amount ranging from about 0.005 wt/v to about 2.5 wt/v ; and a crosslinking agent in an amount ranging from about 0.05 wt/v to about 0.1 wt/v ; or a cellulose nanomaterial in an amount ranging from about 0.1 wt/v to about 10 wt/v ; and an inorganic salt component in an amount ranging from about 0.005 wt/v to about 5 wt/v .
  • the cellulose nanomaterial is selected from cellulose nanofibrils, cellulose nanocrystals, or a combination thereof. In any or all of the described embodiments, the cellulose nanomaterial is present in an amount ranging from about 0.1 wt/v to about 3 wt/v . In any or all of the described embodiments, the inorganic salt component is selected from a sodium-containing salt, a potassium-containing salt, a calcium-containing salt, a magnesium-containing salt, a tin-containing salt, or a combination of two or more thereof.
  • the inorganic salt component is selected from nano calcium carbonate, micro-calcium carbonate, calcium: silicate (90%: 10%), wollastonite, CaCl 2 , NaCl, SnCl 2 , MgCl 2 , KC1, KI, or combinations thereof. In any or all of the described embodiments, the inorganic salt component is present in an amount ranging from about 0.1 wt/v% to about 2 wt/v%.
  • the crosslinking agent is a carboxy- or sulfate - containing polysaccharide selected from alginic acid, sodium alginate, carboxymethyl cellulose, pectic polysaccharides, carboxymethyl dextran, xanthan gum, carboxymethyl starch, hyaluronic acid, dextran sulfate, pentosan polysulfate, carrageenans, fuciodans, or a combination of two or more thereof.
  • the crosslinking agent is present in an amount ranging from about 0.05 wt/v% to about 0.4 wt/v%.
  • the composition can further comprise a stabilizing agent, an additive agent, an agricultural agent, or a combination of two or more thereof thereof.
  • the stabilizing agent is selected from a phenolic compound, an acid, a metal ion, or a combination of two or more thereof;
  • the additive agent is selected from a film forming material, a plasticizer, an antimicrobial agent, an antioxidant agent, a suspension agent/stabilizer, an emulsifier, a mixing aid/defoamer, a preservative, a co-solvent, or a
  • the agricultural agent is selected from nutrients, growth stimulants, plant growth regulators, herbicides, fungicides, pesticides, or a combination of two or more thereof.
  • the composition is formulated for preventing or mitigating pre- and/or post-harvest damage in a plant, fruit, vegetable, or part thereof. In any or all of the described embodiments, the composition is formulated for preventing or mitigating leaching of nutrients, anthocyanins and other biological pigments, or combinations thereof from a plant, fruit, vegetable, or part thereof. In any or all of the described embodiments, the composition is formulated for preventing or mitigating weight loss and UV damage of a plant, fruit, vegetable, or part thereof.
  • the composition comprises cellulose nanofibrils in an amount selected from 0.188%, 0.375%, 0.5 wt/v%, 0.75 wt/v%, 1 wt/v%, 1.5% wt/v%, or 2 wt/v%; nano calcium carbonate in an amount selected from 0.01 wt/v%, 0.05 wt/v%, 0.1 wt/v%, 0.17 wt/v%, 0.38 wt/v%, 0.5 wt/v%, 0.64 wt/v%, 1 wt/v%, 1.5 wt/v%, or 2 wt/v%;
  • Some embodiments concern a plant or plant part comprising a film formed from the composition of any or all of the embodiments described herein.
  • the plant or plant part exhibits reduced weight loss after thawing compared to an equivalent plant or plant part that is not coated with the composition.
  • the plant or plant part exhibits reduced cracking compared to an equivalent plant or plant part that is not coated with the composition.
  • the plant or plant part exhibits reduced anthocyanin leaching, moisture loss, gas exchange, or nutrients loss compared to an equivalent plant or plant part that is not coated with the composition.
  • the plant part is a fruit, a vegetable, or a seed.
  • Also disclosed herein are embodiments of a method comprising substantially coating a plant or plant part with the composition of any or all of the disclosed embodiments before or after the plant or plant part is harvested.
  • the plant or plant part is substantially coated with the composition by spraying, dipping, enrobing, or a combination of two or more thereof.
  • the method further comprises drying plant or plant part after it has been coated to form a film on the plant or plant part, wherein drying involves heating the plant or plant part at a temperature of about 30 °C to about 35 °C.
  • the plant part is a fruit or vegetable.
  • the method further comprises processing the fruit or vegetable to prevent or mitigate leaching of nutrients, anthocyanins and other biological pigments, or combinations thereof in the fruit or vegetable.
  • processing the fruit or vegetable comprises thermally processing the fruit or vegetable at a temperature of at least 80 °C to about 100 °C, using high hydrostatic pressure to process the fruit or vegetable, or combinations thereof.
  • the method further comprises washing the film from the fruit or vegetable before the fruit or vegetable is processed, after the fruit or vegetable is processed, or both. In some embodiments, one or more additional thermal processing steps may be used. In any or all of the described embodiments, the method can further comprise exposing the fruit or vegetable to a processing composition.
  • the processing composition comprises a crosslinking agent in an amount ranging from about 0.01 wt/v to about 0.5 wt/v , an optional sugar compound in an amount ranging from about 12 wt/v to about 25 wt/v , a multivalent salt in an amount ranging from about 1 mM to about 100 mM, or combinations thereof.
  • the processing composition comprises sodium alginate, carboxymethyl cellulose, sucrose, CaCl 2 , or a combination of two or more thereof.
  • the method prevents or mitigates pre- or post- harvest damage of the plant or plant part. In any or all of the described embodiments, the method prevents or mitigates drip loss. In any or all of the described embodiments, the method prevents or mitigates biotic and/or abiotic stress to the plant or plant part. In any or all of the described embodiments, the method prolongs storage or shelf life of the plant or plant part.
  • Some embodiments concern a method, comprising substantially coating a fruit or vegetable before or after it is harvested with a composition comprising a cellulose nanomaterial in an amount ranging from about 0.1 wt/v to about 3 wt/v , an inorganic salt component in an amount ranging from about 0.005 wt/v to about 2.5 wt/v , and a crosslinking agent in an amount ranging from about 0.05 wt/v to about 0.4 wt/v ; drying the composition coating the fruit or vegetable to form a film; thermally processing the fruit or vegetable at a temperature of at least 80 °C to about 100 °C in a processing composition comprising a crosslinking agent in an amount ranging from about 0.01 wt/v to about 0.5 wt/v ; a sugar compound in an amount ranging from about 12 wt/v to about 18 wt/v ; a multivalent salt in an amount ranging from about 5 mM to about 15 mM, or combinations thereof; washing the
  • a nano-cellulose edible coating essentially as described herein may be used.
  • a method of coating an object comprising applying to the object a nano-cellulose coating or coating composition essentially as described herein is provided.
  • cellulose nanocrystal refers to a cellulosic object composed of at least one elementary fibril, containing predominately crystalline and paracrystalline regions, which does not exhibit branches or entanglement between cellulose nanocrystals or network-like structures.
  • cellulose nanofiber refers to a nanofiber predominantly composed of cellulose and exhibiting cellulosic properties.
  • cellulose nanofibril refers to a cellulosic object composed of at least one elementary fibril, containing crystalline, paracrystalline, and amorphous regions, which may exhibit longitudinal splits, entanglement between cellulose nanofibrils, or network-like structure.
  • crosslinking refers to the use of a substance (molecular or ionic) to link at least two molecules (whether the same or different) through a chemical bond, such as a covalent and/or ionic bond.
  • fibril refers to a cellulosic structure, originating from a single terminal enzyme complex, having a configuration of cellulose chains specific to each plant, animal, algal and bacterial species.
  • encapsulation refers to the formation of a complete or partial barrier around a particle or an object for specifically controlling the movement of substances into or out of encapsulated particle or object.
  • exogenous refers to any material that is present in or on an organism or living cell or system or object, but that originated outside of that organism/cell/system/object, as opposed to something that is endogenous. As used herein, exogenous distinguishes the synthetic films disclosed herein from natural films or cuticles produced by plants or plant parts.
  • leaching refers to the extraction of certain organic and inorganic materials from a plant or plant part into a liquid, such as a processing composition or other suitable aqueous or non-aqueous composition.
  • mitigate(ing) refers to the ability of the disclosed composition, a film made from the composition, or a method using the composition to substantially reduce (e.g., such as by about 10%, 20%, 30%, 40%, 50%, 60%, 70%, 80%, or 90%) pre- or post-harvest damage from occurring.
  • pre- or post-harvest damage can be caused by biotic stress, abiotic stress, storage, and/or processing (e.g. , thermal processing).
  • nanofiber as used herein refers to a nano-object with two external dimensions in the nanoscale and the third dimension significantly larger.
  • Nutrients refers to any component that is found in a plant or plant part, whether occurring naturally or having been absorbed during growth. Nutrients can include, but are not limited to primary macronutrients, such as nitrogen, phosphorus, potassium; secondary macronutrients, such as calcium, sulfur, and magnesium; micronutrients or trace minerals, such as boron, manganese, iron, zinc, copper, nickel, and the like.
  • primary macronutrients such as nitrogen, phosphorus, potassium
  • secondary macronutrients such as calcium, sulfur, and magnesium
  • micronutrients or trace minerals such as boron, manganese, iron, zinc, copper, nickel, and the like.
  • plant refers to a whole plant including any root structures, vascular tissues, vegetative tissues and reproductive tissues.
  • a "plant part” includes any portion of the plant.
  • plant parts may be obtained upon harvesting a plant. Plant parts encompassed by the present disclosure include, but are not limited to, flowers, fruits, seeds, leaves, vegetables, stems, roots, branches, and combinations thereof, which are less than the whole plant from which they are derived.
  • pre- or post-harvest damage refers to the ability of the disclosed composition, a film made from the composition, or a method using the composition to completely or substantially stop pre- or post-harvest damage from occurring.
  • pre- or post-harvest damage can be caused by biotic stress, abiotic stress, storage, and/or processing (e.g. , thermal processing).
  • UV damage refers to any sort of damage to the objects described herein that is caused by ultraviolet light.
  • damage can include wilting, discoloration, shrinking, spotting, and the like.
  • compositional components that can be used in the coating compositions, processing compositions, and/or agricultural use compositions disclosed herein are expressed as weight/volume percent unless otherwise indicated.
  • the coating compositions described herein can be prepared using the methods disclosed herein and any other methods known in the art to be suitable for producing a dispersion, solution, or emulsion that can be applied to an object.
  • components of the coating compositions described herein are edible and in some examples they have a regulatory status of generally recognized as safe (GRAS) as provided by the United States Food and Drug Administration. In other examples the components are listed on the Environment Protection Agency's 4A and 4B lists as being safe for the environment.
  • GRAS generally recognized as safe
  • the coating composition can comprise a cellulose nanomaterial.
  • Cellulose nanomaterial is a cellulosic material consisting primarily of linear chains of about one hundred to over ten thousand ⁇ -D-glucopyranose units linked by glucosidic bonds at their CI and C4 positions, with nanoscale external dimensions, or in some embodiments, having nanoscale internal structure or surface structure.
  • cellulose nanomaterials can comprise cellulose nanofibrils (which are also referred to herein as CNF) or cellulose nanocrystals. Such nanomaterials may contain a portion of cellulose microcrystals or cellulose microfibrils.
  • the amount of cellulose microcrystals and/or cellulose microfibrils present in such mixtures can be reduced or increased depending on the extraction method use to make the cellulose nanomaterial and/or by varying the cellulose-containing species from which these components are extracted.
  • the cellulose nanomaterials consist of cellulose nanofibrils or cellulose nanocrystals.
  • the cellulose nanomaterial typically is selected to provide a clear coating and an improved matrix for incorporation of other materials/components disclosed herein.
  • the cellulose nanomaterial of the disclosed coating composition typically is selected to have a suitable structure and suitable chemical properties for use in the particular composition embodiments and methods of using the compositions disclosed herein.
  • the cellulose nanomaterial typically is selected to provide an acceptably clear, water-resistant coating.
  • the cellulose nanomaterial structure and compound properties are optimized to provide a type of cellulose nanomaterial that comprises both crystalline regions and amorphous regions.
  • the cellulose nanomaterial can have dimensions of from about 3 nm to about 300 nm in width.
  • the cellulose nanomaterial can have a length ranging from about 50 nm to about 100,000 nm, such as about 100 nm to about 10,000 nm, about 100 nm to about 5,000 nm, about 100 nm to about 2,500 nm, about 100 nm to about 2,000 nm, or about 100 nm to about 1,000 nm.
  • the disclosed cellulose nanomaterial disclosed herein can have an aspect ratio reminiscent of elementary fibrils in plant cell walls.
  • the cellulose nanomaterial has an aspect ratio ranging from about 10 to about 1 x 10 6 , such about 20 to about 1 x 10 5 ' about 30 to about 1 x 10 4 , about 40 to about 100, or about 50 to about 100.
  • the cellulose nanofibril material disclosed herein is the cellulose nanofibril material disclosed herein.
  • the cellulose nanomaterial can have an aspect ratio ranging from about 5 to about 100, such as about 5 to about 50, about 5 to about 25, about 5 to about 20, about 5 to about 15, or about 5 to about 10.
  • An exemplary cellulose nanomaterial having an aspect ratio within this range is the cellulose nanocrystal material disclosed herein.
  • the cellulose nanomaterial may be cellulose nanofibrils that can be prepared using typical methods known to a person of ordinary skill in the art, such as fibrillation with or without chemical pretreatment in the mechanical refining of cellulose derived from wood fiber or non-wood plant fiber.
  • the method used to prepare the cellulose nanofibrils may or may not provide a composition of cellulose nanofibrils containing residual hemicelluloses.
  • the cellulose nanofibrils may be purchased from a commercial source and then used in the disclosed compositions.
  • the disclosed coating composition also can include one or more inorganic salt components.
  • the inorganic salt component should be suitable for consumption.
  • the inorganic salt component may be added to embodiments of the coating composition to promote UV protection of the object being coated with the coating composition, to increase film strength, film adhesion to the object being coated with the coating composition, and/or complex with components contained within the object being coated.
  • the inorganic salt component may be a nanoparticle or a nano-powder.
  • the inorganic salt component may have a particle size ranging from about 60 nm to about 100 nm, the particle size being determined using Scanning Electron Microscopy (SEM).
  • the inorganic salt component may be selected from any of those typically used in the art as agricultural additives, drug delivery components (e.g. , nano calcium carbonate, which may be loaded with hydrophilic protein-based drugs), or those used for imaging, biomedical and bioscience applications, or as coatings, plastics, nanowires, or alloy and/or catalytic applications.
  • the inorganic salt component is not susceptible to oxidation.
  • the inorganic salt component comprises at least one monovalent or multivalent (such as divalent, trivalent, or tetravalent) ion and a suitable counter-ion.
  • the inorganic salt compound may be selected from sodium-containing salt, a potassium-containing salt, a calcium-containing salt, a magnesium-containing salt, a tin-containing salt, or a combination thereof.
  • Such salts can comprise any suitable counter-ion, such as those that are safe for consumption.
  • Suitable inorganic salt components are selected to maintain the transparency of the film made using the disclosed coating composition and can include, but are not limited to calcium salts (e.g., nano calcium carbonate, a nano calcium silicate compound, such as wollastonite or a combination of calcium and silicate at a ratio of 90%: 10%, respectively, calcium chloride, sodium chloride, and the like), tin salts (e.g. , stannous chloride and the like), magnesium salts (e.g. , magnesium chloride and the like), potassium salts (e.g. , potassium chloride, potassium iodide, and the like), or combinations thereof.
  • calcium salts e.g., nano calcium carbonate, a nano
  • Embodiments of the coating composition disclosed herein can be formulated using various amounts of the disclosed components in any combination.
  • nanomaterial that is used in the coating composition may range from about 0.1% to about 10%, such as about 0.1% to about 5%, about 0.1% to about 3%, about 0.15% to about 2.5%, about 0.19% to about 2%, about 0.25% to about 1.5%, about 0.3% to about 1%, or from about 0.5% to about 1%.
  • Exemplary amounts of the cellulose nanomaterial include about 0.188%, 0.375%, 0.5%, 0.75%, 1%, 1.5%, and 2%.
  • the amount of the inorganic salt component that is used in the coating composition may range from about 0.005% to about 5%, such as about 0.005% to about 2.5%, such as from about 0.05% to about 2%, or from about 0.1% to about 2%, or from about 0.5% to about 2%, or from about 1 % to about 2%, or from about 1.5% to about 2%.
  • Exemplary amounts of the inorganic salt component that can be used in the coating composition include about 0.01%, 0.05%, 0.1%, 0.17%, 0.38%, 0.5%, 0.64%, 1%, 1.5%, and 2%.
  • Certain embodiments of the coating composition need not comprise the inorganic salt component and instead consist of the cellulose nanomaterial.
  • the ratio of the cellulose nanomaterial to the inorganic salt component may range from about 50:50 (cellulose nanomateriakinorganic salt component) to about 99: 1 (cellulose nanomateriakinorganic salt component), with exemplary ratios including 50:50, 99.34:0.66, 96.77:3.23, 93.75:6.25, 90: 10, 80:20, 75:25, 70:30, or 60:40 (cellulose
  • nanomateriakinorganic salt component
  • Exemplary coating composition embodiments disclosed herein can comprise combinations of cellulose nanofibrils, nano calcium carbonate, calcium chloride, sodium chloride, and/or stannous chloride.
  • the amounts of each of these components can be as disclosed herein and these compositions also may comprise one or more additional components discussed below.
  • Some embodiments of the disclosed coating composition may further comprise one or more stabilizing agents.
  • Stabilizing agents may be used to stabilize and retain anthocyanins in plants or a plant part (e.g., fruits or vegetables) during processing to provide for enhanced shelf life, storage, and consumer appeal.
  • Examples of the stabilizing agents that can be added to the disclosed coating composition include, but are not limited to, phenolics, acids, crosslinking agents, metal ions, and combinations thereof.
  • phenolic compounds examples include, but are not limited to, tannic acid, salicylic acid, vanillin, ethyl vanillin, gallic acid, ellagic acid, methyl parabens, propyl parabens, ethyl parabens, butyl parabens, vanillin, butylated hydroxyanisole, butylated
  • Suitable acids include, but are not limited to, formic acid, citric acid, acetic acid, fumaric acid, lactic acid, malic acid, phosphoric acid, tartaric acid, propionic acid, and the like.
  • the acid compound may be the same as a crosslinking component disclosed herein.
  • Crosslinking agents can be added to the composition to improve the material properties, particularly mechanical properties of the films formed from the coating composition, and also the affinity between the cellulose nanomaterial and the inorganic salt component. Without being limited to a single theory of operation, it is currently believed that the crosslinking agent enhances the attraction between the cationic particles of the inorganic salt component and the anionic portions of the cellulose nanomaterial by increasing the degree of anionicity of the cellulose nanomaterial.
  • Crosslinking agents can include, but are not limited to, carboxy- or sulfate- containing polysaccharides. Suitable carboxylated polysaccharides include, but are not limited to, alginic acid (or a salt there, such as sodium alginate), carboxymethyl cellulose, pectic
  • polysaccharides carboxymethyl dextran, xanthan gum, carboxymethyl starch, or combinations thereof.
  • Suitable sulfated polysaccharides include, but are not limited to, hyaluronic acid, dextran sulfate, pentosan polysulfate, carrageenans, fuciodans, or combinations thereof.
  • any suitable non-carboxylated or non-sulfated polysaccharides known in the art can be modified chemically to include these functional groups. In some embodiments, even the cellulose nanomaterial can be functionalized using such methods, such as carboxymethylation of CNF. Such modified polysaccharides also can be used in the disclosed compositions.
  • the crosslinking agent can be an inorganic crosslinking agent, such as sodium trimetaphosphate, calcium acetate, calcium chloride, zinc chloride, magnesium chloride, ferric chloride, manganese, and the like.
  • Organic crosslinking agents (other than the polysaccharides disclosed above) also can be used, such as pyruvic acid, glutaraldehyde, glyceraldehyde, formaldehyde, magnesium and zinc salts of acetic acid, or combinations thereof.
  • FIG. 1A An exemplary embodiment of the disclosed composition is provided in FIG. 1A, which illustrates compositional components and how each component can affect the properties of other components in the composition to provide a durable, water resistant film suitable for the uses disclosed herein.
  • Metal ions may also be added the disclosed compositions to increase the degree of cationicity of the monovalent or multivalent metal present in the inorganic salt component thereby improving the affinity between the inorganic salt component and the cellulose nanomaterial.
  • Metal ions that can be included in the disclosed coating composition include, but are not limited to, calcium (derived from CaCl 2 , for example), tin (derived from food-grade stannous (Sn) chloride, for example), or other food grade metal ions.
  • Amounts of the stabilizing agents that may be used in the disclosed coating composition can be varied to increase and/or decrease a desired property of the coating composition.
  • Phenolic compounds and acids can be present in an amount ranging from 0 to about 5%, such as about 1% to about 5%, or about 2% to about 5%, or about 3% to about 5%, or about 4% to about 5%.
  • Crosslinking agents can be present in an amount ranging from 0 to about 1%, such as about 0.05% to about 1%, about 0.05% to about 0.9%, about 0.05% to about 0.8%, about 0.05% to about 0.7%, about 0.075% to about 0.6%, about 0.1% to about 0.5%, about 0.15% to about 4%, or about 0.2% to about 0.3%, or about 0.25% to about 0.3%.
  • a crosslinking agent may be present in an amount ranging from 0 to 0.5%, such as about 0.05% to about 0.4%, about 0.1% to about 0.3%, or about 0.1% to about 0.25%. Exemplary amounts of the crosslinking agent are selected from 0.05%, 0.1%, 0.15%, and 0.25%.
  • the metal ion can be present in an amount ranging from about 0.5 mM to about 15 mM, such as about 1 mM to about 10 mM, such as about ImM to about 9 mM, or about 1 mM to about 7 mM, or about 1 mM to about 7 mM, or about 1 mM to about 3 mM.
  • the coating composition can further comprise one or more additive agents that when applied to the object to be coated can protect the object from (and/or reduce) water loss, UV damage, and/or loss of physical integrity, all of which are responsible for significant quality deterioration, microbial spoilage and monetary losses to the food industry.
  • suitable additive agents include, but are not limited to, film forming materials, such as chitosan, protein, or a fruit or vegetable puree; plasticizers (such as, but not limited to, glycerin, propylene glycol, sorbitol solutions, sorbitan monostearate, sorbitan monoleate, lactamide, acetamide DEA, lactic acid, polysorbate 20, 60 and 80, polyoxyethylene-fatty esters and ethers, sorbitan-fatty acid esters, polyglyceryl-fatty acid esters, triacetin, dibutyl sebacate, or combinations thereof); antimicrobial agents or antioxidant agents, which can be selected from suitable essential oils (including, but not limited to thyme oil, clove oil, oregano, lemongrass, marjoram, cinnamon, coriander, or combinations thereof), and other suitable components disclosed herein that also exhibit antimicrobial and/or antioxidant activity; suspension agents/stabilizers (including, but not limited to xanthan gum, guar gum,
  • preservatives including, but not limited to sorbic acid, benzoic acid, and salts thereof; nitrates
  • certain additional components can serve multiple purposes in the composition.
  • some additive components such as preservatives and chitosan, can exhibit antimicrobial and/or antioxidant activity, as can certain stabilizing agents, such as acids, and phenolic
  • plasticizers can be present in an amount ranging from 0 to about 10%, such as about 0.1% to about 10%, about 0.2% to about 9%, about 0.3% to about 8%, about
  • the amount of chitosan present may range from about 0 to about 2%, such as about 0.1% to about 1.5%, about 0.2% to about 1%, about 0.3% to about 0.9%, about 0.4% to about 0.8%, or about 0.5% to about 0.7%.
  • the amount of the essential oil present may range from about 0 to about 4%, such as about 0.1% to about 2.5%, about 0.2% to about 1.5%, about 0.3% to about 1.5%, about 0.4% to about 1.5%, or about 0.5% to about 1.5%.
  • agricultural use compositions comprising at least one of the composition components described herein and further comprising one or more agricultural agents selected from nutrients (e.g. , fertilizers), growth stimulants, plant growth regulators, herbicides, fungicides, pesticides, or combinations thereof.
  • the agricultural use compositions, or films made using the agricultural use composition can be made using any of the methods disclosed herein and can applied onto crops, trees, bushes, vines, vegetable plants, ornamental and decorative plants, such as plants grown for their flowers (e.g., roses, carnations, lilies, and so forth) or for their decorative foliage (e.g. , ivy, ferns, and so forth), and the like.
  • the amount of agricultural agent used in the disclosed agricultural use composition may be selected to be within the limitations set forth in EPA guidelines. A person of ordinary skill in the art would recognize that such amounts can be determined by reviewing the EPA guidelines concerning the selected agricultural agent and selecting an amount within the lower and upper limits provided therein.
  • the agricultural agent typically is provided in an amount ranging from about 1 ppm to about 5,000 ppm, such as about 1 ppm to about 4,000 ppm, about 1 ppm to about 3,000 ppm, about 1 ppm to about 2,000 ppm, or about 1 ppm to about 1,000 ppm. Amounts less than or equal to a manufacturer' s suggested application level also may be used and would be readily recognized by those of ordinary skill in the art.
  • compositions disclosed herein include processing compositions, which can be used in combination with the coating compositions disclosed herein.
  • the processing compositions typically are used in methods where the object coated with the disclosed coating compositions undergoes thermal processing.
  • Suitable processing compositions comprise at least one component capable of promoting surface encapsulation of the object being coated, and/or enhancing the thermal stability of one or more pigment components present in the object (e.g. , with a plant or plant part).
  • the processing composition components can chemically interact (e.g. , electrostatically, covalently, and/or ionically) with one or more coating composition components.
  • the processing composition can comprise a crosslinking agent as disclosed herein.
  • crosslinking agents include, but are not limited to, carboxy- or sulfate-containing polysaccharides.
  • Suitable carboxylated polysaccharides include, but are not limited to, alginic acid (and salts thereof), carboxymethyl cellulose, pectic
  • polysaccharides carboxymethyl dextran, xanthan gum, carboxymethyl starch, or combinations thereof.
  • Suitable sulfated polysaccharides include, but are not limited to, hyaluronic acid, dextran sulfate, pentosan polysulfate, carrageenans, fuciodans, and combinations thereof.
  • any suitable non-carboxylated or non-sulfated polysaccharides known in the art can be modified chemically to include these functional groups. Such modified polysaccharides also can be used in the disclosed compositions.
  • the amount of crosslinking agent present in the processing is not limited to, hyaluronic acid, dextran sulfate, pentosan polysulfate, carrageenans, fuciodans, and combinations thereof.
  • any suitable non-carboxylated or non-sulfated polysaccharides known in the art can be modified chemically to include these functional groups. Such modified polysaccharides
  • composition can range from about 0.01% to about 0.5%, such as about 0.01% to about 0.4%, about 0.05% to about 0.3%, about 0.1% to about 0.25%, or about 0.15% to about 0.2%.
  • amount of the crosslinking agent used is about 0.25%.
  • the processing composition can further comprise a sugar compound.
  • the sugar compound is optional and need not be present in the processing
  • the sugar compound is selected from any sugar compound having a brix value of about 12 to about 18.
  • Exemplary embodiments use sucrose, but other similar sugar compounds can be used.
  • the amount of sugar compound used in the processing composition can range from 0 to about 25%, such as about 5% to about 20%, about 12% to about 18%, such as about 12% to about 17%, about 12% to about 16%, about 12% to about 15%, or about 12% to about 14%. In exemplary embodiments, the amount of the sugar compound used is about 18%.
  • processing composition components include, but are not limited to, any of the multivalent salts disclosed herein.
  • the processing solution can include a calcium-containing salt, a magnesium-containing salt, a tin-containing salt, or a combination thereof.
  • An exemplary multivalent salt used in particular working embodiments disclosed herein is CaCl 2 , but other such salts know to those of ordinary skill in the art could be used.
  • the multivalent salt is provided in an amount of about 1 mM to about 100 mM, such as about 5 mM to about 75 mM, about 5 mM to about 50 mM, about 5 mM to about 25 mM, about 5 mM to about 20 mM, about 5 mM to about 12.5 mM, or about 5 mM to about 10 mM.
  • the about of the multivalent salt used is about 10 mM.
  • processing compositions comprising sodium alginate (also referred to as "SA") were used to promote encapsulation of nutrients, pigments, anthocyanins, and the like on the surface of fruit. It is currently believed that this encapsulation is achieved by a chemical crosslinking interaction between the sodium alginate and one or more positively charged ions present in the composition, such as in the form of the inorganic salt component and/or a metal ion additive.
  • SA sodium alginate
  • the sodium alginate-containing processing solutions can therefore also improve the adhesiveness of the coating composition to the surface of coated fruits. The coated fruits therefore become more durable under aqueous conditions, thermal conditions, and other processing conditions.
  • FIG. IB A schematic diagram illustrating a particular embodiment of the disclosed coating composition in combination with the processing compositions disclosed herein is provided in FIG. IB.
  • Processing solutions also can comprise carboxymethyl cellulose (alone or in combination with sodium alginate) to further prevent leaching of nutrients, anthocyanins and other biological pigments from fruits.
  • carboxymethyl cellulose or any other crosslinking agent disclosed herein
  • the carboxymethyl cellulose or any other crosslinking agent disclosed herein
  • the carboxymethyl cellulose further induces metal-complex formation between one or more positively charged ions present in the coating composition (such as those present in the inorganic salt component and/or a metal ion additive) and anthocyanins present in the fruit.
  • An exemplary embodiment is described in FIG. IB.
  • This metal- complex formation can promote polymerization and/or structural modification of anthocyanins present in the fruit.
  • These polymerized or structurally modified anthocyanins are typically more stable and therefore are not degraded and/or leached from the fruit during thermal processing and/or storage.
  • films that can be made using the disclosed composition. Certain embodiments of the disclosed films need not comprise any waxes, oils, or other solvents to be applied to an object.
  • the film can be edible as the film, or composition used to form the film can be formulated with ingredients which are commonly found in food (e.g. , cellulose, calcium carbonate, water, glycerin, etc.) thereby avoiding consumer concerns over food safety.
  • the film may be fibrous or crystalline and can form a durable, inert, water-resistant coating over the object being coated.
  • the composition can be used to form a film over an object, the film having the physical and chemical properties discussed herein.
  • the disclosed compositions also can be used to form flexible packages.
  • Flexible packages include, but are not limited to, biodegradable products, such as boards, films, and packages, or protective coatings.
  • film or coating refers to a layer of the composition created on the exterior of a plant or plant part. The layer need not have a uniform thickness or be completely homogenous in composition. Also, the film or coating need not cover the entire object to which it is applied. In some embodiments, the film or coating can substantially coat the object.
  • the film or coating can cover about 10%, 20%, 30%, 40%, 50%, 60%, 70%, 80%, or 90% of the surface area of the object. In other embodiments, the film or coating can completely coat the object - that is it can cover about 100% of the object. In some embodiments, the film or coating can have a thickness that varies by about 10%, 20%, 30%, 40%, 50%, 60%, 70%, 80%, or 90% over the object.
  • Films and/or flexible packages made from embodiments of the disclosed composition are extremely water resistant and strong. Films and flexible packages comprising combinations of the disclosed composition and other existing film forming materials (such as chitosan, protein, and fruit/vegetable puree) can provide water resistance and barrier properties while retaining the unique functionality of the non-cellulose components of the composition.
  • the films or coatings described herein provide protection from water loss caused by transpiration and/or freeze-thaw related drip loss, and allow for improved water resistance and barrier properties while retaining the unique functionality of the non-cellulose components of the composition.
  • the disclosed compositions When applied to the target surface of plants, plant parts, foodstuffs, animal tissues and inorganic materials, the disclosed compositions form a strong external barrier after drying.
  • the compositions may be dried to form the films by allowing the water in the composition to evaporate.
  • the films are dried using heat to facilitate faster drying of the composition thereby preventing or mitigating long-term exposure to oxygen and light.
  • Temperatures ranging from about 30 °C to about 35 °C can be used to dry the compositions after they have been applied to an object.
  • the films or coatings produced using embodiments of the disclosed compositions can mitigate the loss of color appearance and physical integrity associated with the leaching of anthocyanins and other biological pigments (e.g.
  • compositions, and films made using the compositions can be used to prevent such water loss in susceptible plants, foodstuffs, as well as in animal tissues and inorganic materials.
  • a plant or plant part that comprises a film made from the compositions disclosed herein exhibits properties that would not be exhibited by an equivalent plant or plant part (i.e., an identical unmodified plant or plant part) that does not comprise such a film.
  • the plant or plant part that comprises a film formed from the disclosed composition exhibits reduced weight loss (such as a 10%, 20%, 30%, 40%, 50%,
  • the plant or plant part comprising a film made from the composition disclosed herein exhibits reduced cracking (such as a 10%, 20%, 30%, 40%, 50%, 60%, 70%, 80%, 90%, or 100% reduction) compared to an equivalent plant or plant part that is not coated with the composition.
  • the plant or plant part comprising a film made from the disclosed composition exhibits reduced anthocyanin leaching, moisture loss, gas exchange, or nutrients loss (such as a 10%, 20%, 30%, 40%, 50%, 60%, 70%, 80%, or 90% reduction) compared to an equivalent plant or plant part that is not coated with the composition.
  • the method of making the disclosed composition may comprise dispersing in water (which may be deionized, purified, and the like) a suitable amount of each composition component disclosed herein.
  • both components may be added to water simultaneously.
  • each component may be added sequentially to the same aqueous solution.
  • separate aqueous solutions of each component may be prepared and then mixed together.
  • Other components may be added to the solution containing the cellulose nanomaterial either prior to or after the inorganic salt component is added to the cellulose nanomaterial.
  • Certain components may not need to be dispersed in water prior to mixing and therefore may be added neat to one or more solutions containing other components.
  • mixing can be accomplished by any means known in the art.
  • compositions described herein can form a dispersion, a solution, or an emulsion.
  • exemplary methods of making the composition concern dispersing the cellulose nanomaterial in water and then adding the inorganic salt component to the solution of the cellulose nanomaterial.
  • the solution is then homogenized using a homogenizer at low or high shear.
  • the level of shear used can be modified according to the type of coating composition used.
  • the solution typically is homogenized for a time period suitable for completely dissolving, dispersing, and/or emulsifying the components in water at ambient temperature.
  • one or more of a stabilizing agent, an additive agent, and/or an agricultural agent may be added after the solution of the cellulose nanomaterial and the inorganic salt component before or after the aqueous solution comprising these components has been homogenized.
  • compositions also could be added to separate aqueous solutions of either one of the cellulose nanomaterial and/or inorganic salt component before the two aqueous solutions are combined.
  • the final composition may then be formulated for administration by soaking, spray coating, dipping, enrobing, or any other suitable technique for applying the composition to an object as disclosed herein.
  • the composition is not intended for immediate use, for example when the composition is packaged for future sale.
  • Such compositions are shelf stable, such that less than 20%, 30%, 40% or 50% of the composition will separate after 5, 10, 20, 30 or 60 days of storage. Even longer periods of storage are also contemplated.
  • methods of making shelf-stable compositions can involve choosing appropriate stabilizers to be added to the composition.
  • the composition can be applied relatively soon after mixing.
  • the cellulose nanomaterial can be dispersed in water and then mixed with one or more of the other components at a later time.
  • the cellulose nanomaterial can be dispersed in water with the inorganic salt component to form a pre-mixture, which can be mixed with a separate composition comprising one or more of the stabilizing agents, additive agents, and/or an agricultural agent disclosed herein. The resulting compositions can be then mixed on or near the location where application will occur, thus eliminating the need to create a shelf stable composition.
  • compositions described herein can be used for one or more purposes.
  • One of ordinary skill in the art will appreciate that the methods used to apply the compositions to a subject, plant, or plant parts may vary depending upon the intended purpose of the composition. Additional uses for edible coatings, other than those expressly disclosed herein, will be recognized by those of ordinary skill in the art.
  • compositions disclosed herein can be used to prevent pre- and post-harvest damage to plants, or parts thereof, thus extending shelf-life and increasing marketability of fresh produce.
  • the compositions also can be used in foodstuffs to promote storage and the appearance of food items.
  • the compositions further have uses that are not related to food, but can concern animal healthcare and medical applications.
  • the utility of the disclosed compositions, and films made using such compositions is not limited solely to those described herein.
  • the coating compositions disclosed herein can be easily removed prior to sale or simply peeled away by the consumers.
  • the coating and processing compositions disclosed herein can be used to reduce and prevent anthocyanins and other biological pigments (e.g., betalains) and nutrients leaching from fruits and/or vegetables.
  • anthocyanins and other biological pigments e.g., betalains
  • nutrients can be leached from the fruit into the surrounding aqueous media, which typically is water or a sugar solution, causing a change in appearance (loss of natural fruit pigments) and possible nutritional losses.
  • Composition embodiments disclosed herein can mitigate these losses.
  • the disclosed compositions also are useful as food coatings and in preparation of frozen foods to prevent drip loss and in maintain integrity during thawing.
  • the disclosed compositions can be used to reduce water loss/gain in bakery goods (e.g. , cookies, pastries, and breads) during storage (cold or ambient). Some embodiments can be used to reduce water loss/gain and/or sticking of candies and other confections during storage (cold or ambient). In yet other embodiments, the disclosed compositions can be used to reduce gas (e.g. , 0 2 and C0 2 ) exchange or exposure to harmful gasses (e.g., ethylene gas) of various foods or other organic materials with air in the environment during storage and while on the shelf.
  • gas e.g. , 0 2 and C0 2
  • harmful gasses e.g., ethylene gas
  • compositions disclosed herein can also be used in an agricultural context to protect plant parts (e.g. , agricultural crop seeds), plants and/or plantlets against biotic and/or abiotic stresses prior to and after harvesting.
  • the compositions described herein can be used alone or can be combined with one or more agricultural agents to inhibit biotic stresses, such as insect, nematode, and/or microbial infestation, and also to resist abiotic stresses, such as environmental stresses.
  • biotic stresses such as insect, nematode, and/or microbial infestation
  • abiotic stresses such as environmental stresses.
  • CFUs colony forming units
  • the number of insects or insect larvae can be counted and plant parts (e.g., agricultural crop seeds), plants and/or plantlets that have been treated with the compositions described herein can be compared to similar plant parts (e.g. , agricultural crop seeds), plants and/or plantlets in the same geography that have not been treated.
  • plant parts e.g., agricultural crop seeds
  • plants and/or plantlets in the same geography that have not been treated.
  • the treated plants will display 10%, 20%, 30%, 40%, 50%, 60%, 70%, 80%, or 90% less microbial, nematode, and/or insect infestation compared to control plant parts (e.g. , agricultural crop seeds), plants and/or plantlets.
  • the coating compositions are used to prevent or mitigate abiotic stresses, such as UV light exposure, wind exposure, and low and high temperature exposure, to name a few. Solely by way of example, embodiments of the disclosed composition can be used to prevent cracking in fruit (e.g. , cherries and the like) associated with the water balance of fruits and/or vegetables. Depending on the coating formulation, a 50% to 100% reduction in cracking can be obtained.
  • abiotic stresses such as UV light exposure, wind exposure, and low and high temperature exposure
  • compositions also provide the safe, visibly transparent films that do not impart any significant odor or taste to the foods and that also prevents discoloration or other damage of the fruit caused by UV exposure.
  • the films also can prevent against moisture loss caused by heat and/or sunlight.
  • the coating compositions described herein are also useful in post handling of animal tissues, healthcare and related medical applications, to protect (that is, reduce the effects of) the body and especially the skin from damage due to moisture loss, UV light exposure, heat, and other biotic and/or abiotic stresses. Exposure to high levels of UV light can damage maturing produce, resulting in visibly discolored spots, destroying phytochemical compounds, and providing a foothold for spoilage organisms to grow.
  • compositions Modifying the physical properties of biodegradable products such as boards, films and packages, for instance to provide increased resistance to degradation, improved barrier properties, and/or improved strength is yet another application for the disclosed compositions. It is also contemplated that the films and compositions provided herein can be used as a protective surface treatment or coating for durable materials, such as to reduce or prevent damage during transit and handling.
  • durable materials such as to reduce or prevent damage during transit and handling.
  • the majority of flexible packaging materials in the food industry are petroleum-derived polymers. Their lack of sustainability and concerns over toxic residues result in decreased appeal to consumers. Alternate natural materials (e.g. , cellulose and chitosan) lack water resistance.
  • the compositions disclosed herein can be used to provide coatings that address these limitations.
  • compositions include, but are not limited to, the particular applications provided in Table 1.
  • cherries and blueberries enables new packaging of these products (for example, the fruit can be displayed in a clear container and retain the appearance of fresh fruit
  • compositions can be selected from:
  • the compositions can be applied as a dispersion, a solution, or an emulsion to any of the objects disclosed herein.
  • Techniques known to those of ordinary skill in the art may be used to apply the compositions to form films.
  • the object may be dipped into a dispersion, a solution, or an emulsion of the composition.
  • a dispersion, solution, or emulsion of the composition may be dripped onto the object.
  • the object may be coated (partially or wholly) by spray-coating a dispersion, a solution, or an emulsion of the composition onto the object.
  • the object also can be enrobed (partially or wholly) using a mechanical applicator to apply a dispersion, solution, or emulsion of the composition to the object.
  • the composition can be added to the object prior to being harvested or after harvesting. Suitable sprayers and enrobers would be recognized by those of ordinary skill in the art.
  • the coating method may be chosen based on the viscosity of the coating composition. For example, if the coating composition is viscous and the object being coated is a post-harvest product (e.g., fruit or vegetable), then dipping or dripping methods of application are typically used. Pre-harvest application typically involves applying the coating to the plant or plant part thereof using a spraying method.
  • compositions are suitable for use with plants or parts thereof (e.g., fruits and/or vegetables) that are exposed to post-harvest treatment.
  • fruits and/or vegetables can be thermally processed to promote the shelf life of the fruit or vegetable, and foodstuffs made using such fruits and vegetables.
  • An example is the thermal processing of fruits or vegetables for preservation.
  • Another example is storing fruits or vegetables at cold temperatures.
  • Yet another example is high hydrostatic pressure (HHP) processing of fruits or vegetables.
  • High hydrostatic pressure processing is a method of processing where products, such as fruits or vegetables, are subjected to elevated pressures (such as about 6,000 atm) with or without the addition of heat to achieve, for example, microbial inactivation or to alter the product attributes to achieve consumer-desired qualities (such as reduced leaching of nutrients,
  • compositions are suitable for use in these processing applications and any other processing technique used in the art.
  • compositions can be used in thermal processing of products disclosed herein.
  • Thermal processing typically involves at least one thermal processing step that comprises exposing a product coated with a film made from the compositions disclosed herein to heat.
  • An exemplary schematic diagram of thermal processing, as disclosed herein, is illustrated in FIG. 2.
  • products can be sorted and washed and coated with a coating composition embodiment disclosed herein. The products are then dried to form a film from the composition and
  • FIG. 2 further illustrates that certain embodiments of the thermal processing method disclosed herein can include a washing step to remove the film and improve the appearance of processed products.
  • the temperature at which the sample is heated can be modified depending on the type of product used and the type of storage solution (e.g. , if a highly acid solution is used to store the fruit, then lower temperatures may be used).
  • the thermal processes disclosed herein involve using temperatures of at least 80 °C to about 100 °C, such as about 90 °C to about 94 °C, or about 91 °C to about 93 °C.
  • a typical thermal processing step is used after the coating composition has been added to and dried onto the product that will undergo processing.
  • the sample may then be heated in water or it may be combined with a processing composition as disclosed herein. Coated samples (with or without) processing compositions can then be heated at an appropriate temperature for a sufficient time period.
  • the sample is heated in the processing solution for at least 5 minutes to about 30 minutes, such as about 10 minutes to about 25 minutes, about 10 minutes to about 20 minutes, or about 10 minutes to about 15 minutes.
  • thermal processing is completed by utilizing at least one thermal processing step that implements commercial canning requirements to ensure product safety.
  • the sample can be heated and simultaneously maintained at a certain pH in a pH-modified processing solution.
  • the processing solution typically is maintained at a pH of at least 4, and may be as high as about 5.5.
  • the pH in some examples can be about 4.5.
  • the pH may be adjusted to accommodate the particular processing temperature used.
  • samples maintained at a pH greater than about 4.6 should be heated at temperatures of at least about 90 °C to avoid contamination (e.g., to prevent causing botulism).
  • Samples that are maintained at lower pH values e.g., below 4.6
  • this particular thermal processing step can be the only thermal processing step.
  • this particular thermal processing step may be combined with one, two, three, or more, prior thermal processing steps wherein the pH of the solution need not be maintained or controlled.
  • the film coating the product may be removed at different stages of thermal processing.
  • the films can be removed by rinsing with water, agitation, exposure to high velocity rinsing sprays, using chemical conditions (e.g. , exposure to acidic or basic solutions, enzymatic treatments, or exposure to other reactive species).
  • the film can be removed after a first thermal process step described above (with or without pH control) to improve the appearance of the processed products.
  • the product can then undergo a suitable final thermal processing step.
  • the film is removed after a first thermal processing step, at which point the product is exposed to a second, subsequent thermal processing step. The product may then be washed and exposed to a final thermal processing step.
  • the film need not be removed and can be included in the final processed product. Removing the film does not require removing all of the film or components thereof. Residual amounts of the film or its various components may remain on the product; however, these residual amounts do not affect the appearance, taste, or quality of the product.
  • Suitable alternative processing methods include high hydrostatic pressure (HHP) processing methods.
  • products e.g., fruits and vegetables
  • HHP high hydrostatic pressure
  • a suitable pressure for a suitable time (typically at ambient temperature), such as at a pressure and for a time that is capable of inactivating harmful microorganisms and enzymes that may lead to quality deterioration and food safety concern of products during storage.
  • exemplary pressures include pressures ranging from about 400 to about 800 MPa, such as from about 400 to about 500 MPa using a high pressure unit.
  • the time may range from greater than about 5 minutes to about 20 minutes, such as about 10 minutes to about 15 min.
  • products are first coated using the coating compositions disclosed herein and then packed in a suitable container, such as a polyethylene terephthalate (PET) retort bowl or other container that can subjected to HHP treatment, such as a polymer cup, glass jar, metal can, or flexible pouch.
  • a suitable container such as a polyethylene terephthalate (PET) retort bowl or other container that can subjected to HHP treatment, such as a polymer cup, glass jar, metal can, or flexible pouch.
  • PET polyethylene terephthalate
  • the products can be packaged in the container with any one of the processing compositions disclosed herein.
  • the samples can be sealed and subjected to a first thermal processing step as disclosed herein, followed by an HHP processing step.
  • the samples are first subjected to a first thermal processing step using a first processing composition prior to being packaged in the container for
  • the samples may then be separated from the first processing composition used in the first thermal processing step and placed into a fresh processing composition, which can be the same or different from the first processing composition.
  • This embodiment may further comprise removing the films or coatings formed on the products after the first thermal processing step.
  • the samples are then processed using an HHP processing step. Any of these embodiments can be modified to include a second thermal processing step after the samples have undergone HHP treatment.
  • the products can be removed from the packaging before or after this second thermal processing step, and any residual film or coating present on the products may also be removed before or after this second thermal processing step.
  • Other disclosed embodiments concern storing foodstuffs, fruits, and/or vegetables coated with a film formed from the disclosed compositions at low temperatures for preservation. These products can be frozen or merely stored in cold temperatures (e.g. , such as temperatures of a cold room, refrigerator, and the like) for long periods of time. Such embodiments need not implement a thermal processing step to obtain the desired film properties.
  • the object can be contacted with embodiments of the composition disclosed herein, thereby providing improved products.
  • the object is a plant or plant part.
  • Exemplary objects include fruits, such as those disclosed in Table 1.
  • the objects comprising a coating or film produced by the composition include components as described herein, but upon drying the relative concentration of the components is altered due, for instance, to the loss of water from the composition. Therefore, the film or coating formed will generally contain less water and higher concentrations/ratios of the (non-evaporative) compositional components.
  • the amounts provided below in Table 2 correspond to representative amounts of components present in the dried film, and are expressed as wt/wt%.
  • Inorganic salt component 0-50% l%-40% l%-20% 1%-10%
  • Stabilizing agent 0-30% 0.5%-20% 1%-15% 1%-10%
  • compositions comprising cellulose nanofibrils (CNF) comprising both crystalline regions and amorphous regions, with dimensions of three to several hundred nm in width, and having an aspect ratio greater than 50, reminiscent of elementary fibrils in plant cell walls.
  • CNF cellulose nanofibrils
  • the CNFs are formed by fibrillation methods with or without chemical pretreatment in the mechanical refining of cellulose such as, but not limited to wood fiber or non-wood plant fiber, and may or may not contain residual hemicelluloses.
  • the CNF was obtained from a commercial source.
  • Nanoparticles, nano dots or nano powder calcium carbonate are cubic, high surface area particles.
  • Nano-sized calcium carbonate has a particle size of about 60 nm to about 100 nm when examined by Scanning Electron Microscopy (SEM).
  • SEM Scanning Electron Microscopy
  • Existing applications for NCC has focused on its use in drug delivery by loading them with hydrophilic protein-based drugs and for their potential imaging, biomedical and bioscience properties and for use in coatings, plastics, nanowire, and in alloy and catalyst applications.
  • the NCC was obtained from a commercial source.
  • Table 4 provides various different formulations of CNF and NCC compositions.
  • the given amount of CNF, NCC, and/or CaCl 2 was dissolved in deionized water and then homogenized using a homogenizer for reaching complete dissolution of the composition components under ambient conditions.
  • This example describes the prevention of pigment/nutrient leaching from blueberry fruits using embodiments of the composition disclosed herein. All embodiments, with and without the addition of nano calcium carbonate, virtually eliminated the leakage of anthocyanin pigments (compared with a control) from blueberries during thermal processing analogous to that seen in the industry.
  • Blueberries were coated with different CNF, NCC, and CaCl 2 solutions as described in Table 4 by either dipping the fruit in a solution of the composition (the blueberries were dipped in a solution of the composition for 1 minute and then dried at room temperature) or spray-coating (a solution of the composition was sprayed on the surface of blueberries under 30 psi pressure and then dried at room temperature).
  • the uncoated and coated blueberries were packed in glass jars filled with distilled water, put inside a water bath with controlled temperature, and then subjected to one of the following thermal process conditions: 1) heating at 80 °C for 20 min; 2) heating at 65 °C for 15 min; and 3) a sequence of conditions (1) and (2).
  • thermal process conditions 1) heating at 80 °C for 20 min; 2) heating at 65 °C for 15 min; and 3) a sequence of conditions (1) and (2).
  • pigment and anthocyanin content in the packing water after thermal processing of the blueberries was determined.
  • the color of packing water was measured using a UV spectrophotometer at 525 nm (Shimadzu, Japan).
  • FIGS. 3A-3E illustrate that the leaching of anthocyanins and other biological pigments was eliminated or greatly reduced by the CNF/NCC compositions (FIGS. 3B-3E), compared with uncoated blueberries (FIG. 3A).
  • the color of the water surrounding the blueberries in FIGS. 3B, 3C, particularly FIG. 3E was less red than the water surrounding the blueberries in FIG. 3 A.
  • FIGS. 4A-4C illustrate that even after the film of the composition was removed after the first thermal treatment (FIG. 4B), pigment leaching was negligible after the second stage of thermal treatment shown in FIG. 4C as the color of the water surrounding the blueberries illustrated in FIG.
  • FIG. 4B was free of color, whereas the water surrounding the blueberries illustrated in FIG. 4C was tinted red. Further, the coating formulations containing NCC showed lower levels of leaching compared to those without as shown in FIG. 5, which illustrates the levels of monomeric anthocyanin and pigments leached from coated or uncoated blueberries after processing (80 °C for 20 minutes) and cooling (20 minutes) and FIG. 6, which illustrates the levels of monomeric anthocyanin and pigments leached from coated or uncoated blueberries after one day of storage.
  • FIGS. 7A-7F and FIG. 8 illustrate that the leaching of anthocyanin pigments from blueberries was significantly reduced by using CNF/CaCl 2 compositions (FIGS. 7D-7F, and indicated as "NF1.5CC” in FIG. 8) after thermal process (80 °C for 20 minutes), compared to uncoated blueberries (FIGS.
  • FIGS. 9 A and 9B illustrate that leaching of anthocyanin pigments was eliminated by the CNF/CaCl 2 compositions disclosed herein (FIG. 9B), as compared with uncoated cherries (FIG. 9A).
  • the water surrounding the cherries illustrated in FIG. 9A turned bright red; whereas the water surrounding the cherries illustrated in FIG. 9B remained colorless.
  • This example describes using embodiments of the composition disclosed herein to coat apples.
  • Apples were peeled, cored and cut into slices of uniform thickness. The resultant slices were then dipped in CNF-containing compositions or left uncoated prior to freezing in a forced air freezer (-20 °C) for 24 hours. Afterwards, the samples were removed from the freezer and allowed to thaw at ambient temperature (18-23 °C) for about 6 hours. Measurements were taken of both the change in mass during freezing (condensation) and the total amount of liquid exuded from the thawing apples (syneresis and evaporation).
  • This example concerns methods to prepare CNF-containing flexible, water-resistant films that are useful when applied as an edible food packaging wrap for a wide variety of food products.
  • compositions comprising CNF (0.188% and 0.375%) were prepared, casted in Teflon- coated glass plate, and dried at room temperature for 72-96 hours (Chen and Zhao, 2012). See, Chen, J. and Zhao, Y., "Effect of molecular weight, acid, and plasticizer on the physicochemical and antibacterial properties of beta-chitosan based films," J. Food Sci. 77(5), E127-136.
  • a composition comprising 1% carboxymethyl cellulose also was prepared to make films as a comparison with the CNF-containing films. Prepared films were conditioned for 48 hours in a 25 °C and 50% relative humidity (RH) environmental chamber.
  • Conditioned film samples were tested for moisture content, water solubility, and water-vapor transmission rate (WVTR), as well as tensile strength and elongation.
  • the moisture content of the films was determined by the percentage weight loss of film samples after drying in a forced-air oven at 100 °C for 24 hours.
  • Water solubility was determined by the percentage weight loss of films samples after suspension in water for 24 hours and dried at 40 °C for 24 hours, whereas the control carboxymethyl cellulose film was only tested for 2 hours due to its hydrophobicity.
  • WVTR was measured by the cup method at 25 °C and 100/50% RH gradient, following ASTM Standard Method E96-87 (ASTM, 2000).
  • Tensile strength (TS) and percent elongation at the break (EL) of the films were each determined according to ASTM D882 (ASTM, 2001) and analyzed using a texture analyzer ( ⁇ . ⁇ 2 ⁇ , Texture Technologies Corp., USA) by following the same procedures as Park and Zhao (2004). See, Park, Su-il, and Yanyun Zhao, "Incorporation of a High Concentration of Mineral or Vitamin into Chitosan-Based Films," Journal of Agricultural and Food Chemistry 52, no. 7 (2004): 1933-1939.
  • This example describes a method for providing UV sunburn protection within CNF/NCC coatings and films before and after harvest.
  • UV protective films with carboxymethyl cellulose and CNF-containing compositions were prepared following the same procedures described above and used to cover the top of cylindrical acrylic vessels containing 10 mL of a buffered liquid dosimetry solution (0.6 M KI, 0.1 M KIO 3 , and 0.01 M Na 2 B 4 O7*10H 2 O). Fluence measurements (mJ/cm ) were obtained by subjecting the vessels to ultra violet light for a fixed time and then measuring the change in the absorbance of the solution at 352 nm, as illustrated in FIG. 12. Transmittance of visible and UV light was also determined using spectrophotometry at 620 nm and 280 nm. Additionally, whole apples (Malus domestica, var.
  • golden delicious were coated with the compositions using either spraying or dipping methods. After the coatings/films had dried, the coated samples and un-coated samples were exposed to a 10W UV source for 1.5 hours to induce UV damage. Samples were stored at ambient temperature for 12 days and periodically assayed for color and weight loss (%), and photographed to record changes in appearance.
  • NCC transmittance
  • FIGS. 15A-15D illustrate results obtained from embodiments where a set of uncoated pears (after 10 days) is illustrated in FIG. 15 A, which illustrates these pears as having little to no discoloration and/or wilting. The same set of pears is illustrated in FIG. 15C, which illustrates the pears after being stored for 25 days under ambient conditions - these pears are significantly discolored (with large brown spots/patches) and wilted.
  • Pears comprising a coating of by 1.5% CNF with 0.1% CaCl 2 are illustrated in FIG. 15B.
  • compositions are capable of preventing or mitigating post-harvest biotic and/or abiotic stresses was conducted using apples.
  • FIGS. 16A and 16B The results of this embodiment are illustrated in FIGS. 16A and 16B.
  • Uncoated apples after being stored for 25 days under ambient conditions are significantly discolored (from red to yellow) by oxidative degradation of color pigments and wilted due to weight loss (FIG. 16A).
  • Apples comprising a coating of by 1.5% CNF with 0.1% CaCl 2 exhibited little to no discoloration and/or wilting (FIG. 16B).
  • aqueous suspension/slurries of fibrous or crystalline nano-cellulose that are capable of forming clear, durable and water-resistant coatings to prevent cherry cracking are provided.
  • These coatings can carry other functional substances, such as nano- calcium carbonate to further enhance its water-resistant function.
  • This example illustrates the ability to protect fresh cherries; however, a person of ordinary skill in the art would recognize that the compositions, films, and methods of making/using such compositions and films is not limited to cherries.
  • the disclosed methods can be used with other objects disclosed herein to decrease cracking, such as that associated with the water balance of fruits and/or vegetables, to enhance the marketability.
  • Table 8 shows a list of formulations of CNF/calcium compositions. To prepare the compositions, the given amount of CNF and/or calcium was dissolved in deionized water and then homogenized for complete dissolution of CNF and calcium at ambient conditions.
  • ⁇ A11 formulations were prepared by dispersing the components in deionized water
  • Uncoated cherries (control) and coated cherries with two different coating solutions were soaked in water for 8 h at room temperature.
  • the numbers of non-cracking and cracking cherries were counted, and the cracking ratio was presented based on the total number of cherries (53 ea.).
  • the weight gain (%) of the cherries was determined as:
  • Weight gain (%) (weight of cherries after soaking for 8 hours - initial weight of cherries) / initial weight of cherries *100.
  • Weight loss (%) (Initial weight of container - weight of container after cherries were soaked for 8 hours) / initial weight of container * 100.
  • Table 9 The number of cracked cherries after 8 h soaking in distilled water.
  • Weight gain of cherries and weight loss of soaking water are provided in FIG. 18. No significant difference in weight gain of cherries was observed between coated and uncoated cherries, but weight gain of cherries coated twice with the NF2 composition was significantly lower than that of control and other coated cherries. The significantly different higher loss of water from container was found in soaking solution treated for NF2C2 coated cherries. This result is likely caused by water absorption by the coating materials.
  • aqueous suspension/slurries of fibrous or crystalline nano-cellulose that are capable of forming optimal concentration of micro calcium carbonate (microCaC0 3 )added to cellulose nanofibrils (CNF) to prevent cherry cracking (and increasing marketability) were examined.
  • microCaC0 3 micro calcium carbonate
  • CNF cellulose nanofibrils
  • the cracking ratio of cherries reduced to 13% in cherries coated with a composition comprising the NF1.5C0.01 formulation and 0% in cherries coated with a composition comprising the NF1.5C0.05, NF1.5C0.1, NF1.5C0.5, and NF1.5C1 compositions.
  • the optimal concentration of micro CaC0 3 ranges between from about 0.05% to about 0.10%.
  • Table 10 The number of cracked cherries after 8 hours soaking in distilled water.
  • FIGS. 20A-20E illustrate results from compositions comprising 1.5% CNF and different concentrations of wollastonite
  • the same formulas disclosed in Example 7 were used to calculate weight gain (%) and weight loss (%).
  • the cracking ratio of cherries reduced 50% in cherries coated with the NF1.5C0.64 (70/30) composition (using wollastonite) and 63.33% in cherries coated with the NF1.5C1 (60/40) composition (using calcium and silicate as 90% and 10%).
  • aqueous suspension/slurries of fibrous or crystalline nano-cellulose that are capable of forming optimal concentration of cellulose nanofibrils (CNF)/calcium chloride (CaCl 2 ) coating for reducing cherry cracking.
  • CNF cellulose nanofibrils
  • CaCl 2 calcium chloride
  • FIGS. 22A-22E reflect the results reported in Table 12, the cracked and un-cracked cherries after soaked in water for 8 hours. Hence, adding 0.1% or 0.5% CaCl 2 to compositions comprising CNF significantly reduced cherry cracking.
  • the total monomeric anthocyanin content of fruit was determined using the pH-differential method and expressed as mg cyanidin-3-glucoside per 100 g dried matter (DM) of fruit with molecular weight of 449.2 g/mol and a molar absorptivity of 26,900.
  • Percent polymeric color (PPC) was calculated as the sum of the absorbance at 420 nm and 520 nm of bisulfite-treated extract divided by the sum of the absorbance at 420 nm and 520 nm of berry extract.
  • FIGS. 24A-24H illustrate results obtained from uncoated blueberries (FIG. 24A) and blueberries coated with a compositions comprising lower concentrations (0.5 and 0.75%) of CNF. Varied amounts of NCC, CMC, and CaCl 2 were used. Blueberries coated with compositions comprising CNF, NCC, and CMC only showed significant less anthocyanin leaching in comparison with those containing CNF, NCC, and CaCl 2 . The results are illustrated in FIGS. 24A-24H, which also are described below in Table 14.
  • coated fruits were thermally processed in two different ways: 1) a one-step thermal process (OTP) at 91-93 °C in a water bath for 9-10 min; and 2) a repeated two-step thermal processes (TTP) at 91- 93 °C for 9-10 min.
  • OTP one-step thermal process
  • TTP repeated two-step thermal processes
  • anthocyanins were polymerized and/or structurally modified under the layer of the film formed by the composition used to coat the fruit in the first thermal treatment. This polymerization and/or structural modification promoted the thermally stability of the fruits in aqueous solutions.
  • the surface coating was then washed after the first thermal process step using water. This washing step was used to improve the appearance of the fruit surface. After rinsing in water, the fruit embodiments were repacked in an aqueous solution containing 0.25% sodium alginate, 0.25% CMC, or 10 mM CaCl 2 and 18% sugar (table sugar) at a pH ranging from about 4.5 to about 5.0.
  • CNF, 0.1% CMC, and 0.5% NCC showed less leaching of anthocyanin pigments in the aqueous solution compared with other coating treatments.
  • the monomeric anthocyanin pigment of the aqueous solution was measured.
  • Significant reduction in pigment leaching were observed on blueberries coated with a composition embodiment comprising 1% CNF, 0.1% CMC, and 0.5% NCC (FIG. 25C), compared with the control (FIG. 25A) and other treatments (FIG. 25B, 25D, and 25E).
  • composition comprising 1% CNF, 0.1% CMC, 0.5% NCC was selected for storage tests.
  • Blueberries coated with this composition embodiment were stored in a processing composition comprising 0.25% sodium alginate and 18% sugar. These embodiments showed less leaching after 7 days of storage at ambient conditions in comparison with blueberries that were not coated with the composition (FIGS. 28A-28C).
  • FIGS. 29A-29E Results from embodiments where blueberries coated with a composition comprising 1% CNF, 0.1% CMC, and 0.5% NCC were added to these other processing compositions are illustrated in FIGS. 29A-29E and are also summarized in Table 15, below.
  • the processing compositions comprised 0.25% CMC and 18% sugar or 0.25% CMC, 18% sugar, and 10 mM CaCl 2 .
  • the blueberries were treated using the two- step of thermal process, and stored at the ambient condition for 7 days. No leaching of anthocyanin pigments was observed at day zero, whereas anthocyanin pigments were leached during storage under ambient conditions. Acidic pH (4.5) condition of aqueous solution showed more leaching of anthocyanin pigments than neutral pH (Fig. 29E).
  • the monomeric anthocyanin pigment of blueberries coated with 1% CNF, 0.1% CMC, and 0.5% NCC was significantly reduced (as compared to controls wherein the fruit was not coated with the composition).
  • the processing compositions comprising sodium alginate used with coated blueberries and that were subjected to a one-step thermal process exhibited the lowest monomeric anthocyanin pigment concentration (FIG. 30).
  • High hydrostatic pressure is a novel non-thermal food processing technology that has shown its effectiveness for retaining the nutritional and sensory qualities of processed fruits while killing harmful microorganisms and inactivating enzymes for ensuring food safety and quality of processing fruit products.
  • This technology has been used in commercial food processing, including processing fruits and vegetables. This technology is suitable for use with the
  • compositions and methods disclosed herein can be used to effectively prevent anthocyanin leaching from fruit packed in aqueous media that is subjected to an HHP process.
  • exemplary compositions include those comprising CNF, nano-CaC0 3 , and CMC.
  • fruits are processed at a suitable pressure for a suitable time, such as at a pressure and for a time that is capable of inactivating harmful microorganisms and enzymes that may lead to quality deterioration and food safety concern of fruit during storage.
  • Exemplary pressures include pressures ranging from about 400 to about 800 MPa, such as from about 400 to about 500 MPa.
  • Exemplary time ranges include from greater than about 5 minutes to about 20 minutes, such as about 10 minutes to about 15 min using a high pressure unit, such as that available at the OSU Food Science pilot plant.
  • fruits such as blueberries, cherries and other anthocyanin rich fruits
  • a suitable container such as polyethylene terephthalate (PET) retort bowls or other types of containers that can subjected to HHP treatment, such as polymer cups, glass jars, metal cans, or flexible pouches and/or bags of polymer or composite manufacture
  • HHP treatment such as polymer cups, glass jars, metal cans, or flexible pouches and/or bags of polymer or composite manufacture
  • the samples are sealed and subjected to a first thermal processing step as disclosed herein, followed by an HHP processing step.
  • the samples are first subjected to a first thermal processing step prior to being packaged in the container. The samples may then be separated from the first processing
  • This embodiment may further comprise removing (using methods disclosed herein) the films or coatings formed on the fruit samples after the first thermal processing step.
  • the samples are then processed using an HHP processing step. Any of these embodiments can be modified to include a second thermal processing step after the samples have undergone HHP treatment.
  • the fruit samples can be removed from the packaging before or after this second thermal processing step, and any residual film or coating present on the fruit samples may also be removed before or after this second thermal processing step.
  • FIG. 31 illustrates a photographic image of uncoated blueberries packed in a polyethylene terephthalate (PET) retort bowl that was subjected to HHP processing. As illustrated in FIG. 31, anthocyanin was leached from the fruits into the packing solution. The compositions disclosed herein are used to prevent the leaching of anthocyanin from HHP-processed fruits.
  • PET polyethylene terephthalate
  • compositions disclosed herein also may be used to with multi-colored fruit products packed in clearly visual containers to promote well retained natural fruit pigments, nutrients and extended shelf-life.
  • composition embodiments disclosed herein can be used to coat mixed fruits, such as blueberries, cherries, and other anthocyanin rich fruits, that are then processed in clear PET cups or glass jars (FIG. 32) except the fruits have been thermally or on- thermally (HHP) processed for ensuring food safety, quality and shelf-life).
  • This example describes use of the disclosed compositions on apples, grapes, and certain tropical fruits.
  • the fruits described below were coated with an embodiment of the composition and stored under ambient conditions.
  • FIG. 33 illustrates the weight loss of uncoated (control) and 1.5% cellulose nanofibrils (CNF)/0.1% nano calcium carbonate (NCC) coated apples, mangoes, and grapes during 14 days of storage under ambient conditions. There was no significant difference of weight loss (%) between uncoated and coated-apples and grapes, whereas the weight loss of coated-mango was significantly reduced in comparison with that of uncoated mango in 8, 11, and 14 days of storage.
  • CNF cellulose nanofibrils
  • NCC nano calcium carbonate
  • coated mangoes were covered with a film made from two different coating compositions, 1.5% cellulose nanofibrils (CNF)/0.1% nano calcium carbonate (NCC) or 1.5% CNF/0.1% NCC/0.1% carboxymethyl cellulose (CMC). Each coating composition was applied by spray coating.
  • CNF cellulose nanofibrils
  • NCC nano calcium carbonate
  • CMC carboxymethyl cellulose
  • 36B which illustrates grapes coated with a composition comprising 1.5% CNF, 0.1% NCC, and 2.5% CLE
  • 36C which illustrates grapes coated with a composition comprising 1.5% CNF, 0.1% NCC, 0.1% CMC, and 2.5% CLE.
  • the white materials observed in the film of the coated grapes can be removed by a suitable washing process.
  • Coated papaya treatment A, showed significantly lower weight loss in comparison with a control papaya (no coating) after 3 days of storage under ambient conditions. No significant decrease of weight loss was observed in coated citrus fruits after 5 days of storage at the ambient condition (FIG. 37).

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  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
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  • Health & Medical Sciences (AREA)
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  • Jellies, Jams, And Syrups (AREA)
  • Paints Or Removers (AREA)

Abstract

La présente invention concerne des modes de réalisation d'une composition comprenant au moins une nanomatière cellulosique et un constituant sel inorganique. Les compositions de l'invention sont utiles pour former des revêtements/films comestibles sur des plantes, des parties végétales et d'autres objets. Dans certains modes de réalisation de l'invention, les compositions comprennent en outre un agent de réticulation. Les compositions et revêtements/films de l'invention obtenus à l'aide des compositions sont efficaces pour la protection de produit frais et traité et d'autres substances et produits, à partir d'une diversité de différents types d'endommagement de traitement d'aliment (et les effets nocifs associés à ceux-ci) et de stress biotiques et/ou abiotiques qui réduisent la qualité et la commercialité.
EP14769964.9A 2013-03-14 2014-03-14 Revêtements comestibles de nano-cellulose et leurs utilisations Withdrawn EP2967093A1 (fr)

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CL2015002660A1 (es) 2016-03-04
AU2014236213A1 (en) 2015-11-05
WO2014153210A1 (fr) 2014-09-25
BR112015023436A2 (pt) 2017-07-18
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MX2015012706A (es) 2016-06-14
KR20230022454A (ko) 2023-02-15

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