WO2023192594A1 - Poudres de composé actif séché par pulvérisation électrostatique et leur procédé de production - Google Patents

Poudres de composé actif séché par pulvérisation électrostatique et leur procédé de production Download PDF

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Publication number
WO2023192594A1
WO2023192594A1 PCT/US2023/017101 US2023017101W WO2023192594A1 WO 2023192594 A1 WO2023192594 A1 WO 2023192594A1 US 2023017101 W US2023017101 W US 2023017101W WO 2023192594 A1 WO2023192594 A1 WO 2023192594A1
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WIPO (PCT)
Prior art keywords
oil
active compound
powder
powders
ester
Prior art date
Application number
PCT/US2023/017101
Other languages
English (en)
Inventor
Bogdan Zisu
Akm MASUM
Bao Loc PHAM
Michel Thenin
Audrey MAUDHUIT
Elodie BEAUPEUX
Thomas Elliot Ackerman
Jason Tyler RUSCH
Lyndon John Wee Sit
Original Assignee
Sppraying Systems Co.
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.)
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Publication date
Priority claimed from PCT/US2022/054149 external-priority patent/WO2023129587A1/fr
Application filed by Sppraying Systems Co. filed Critical Sppraying Systems Co.
Priority claimed from US18/129,355 external-priority patent/US20230240314A1/en
Publication of WO2023192594A1 publication Critical patent/WO2023192594A1/fr

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Classifications

    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23P—SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
    • A23P10/00—Shaping or working of foodstuffs characterised by the products
    • A23P10/30—Encapsulation of particles, e.g. foodstuff additives
    • A23P10/35—Encapsulation of particles, e.g. foodstuff additives with oils, lipids, monoglycerides or diglycerides
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
    • A23D9/00—Other edible oils or fats, e.g. shortenings, cooking oils
    • A23D9/007—Other edible oils or fats, e.g. shortenings, cooking oils characterised by ingredients other than fatty acid triglycerides
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
    • A23D9/00—Other edible oils or fats, e.g. shortenings, cooking oils
    • A23D9/02—Other edible oils or fats, e.g. shortenings, cooking oils characterised by the production or working-up
    • A23D9/04—Working-up
    • A23D9/05—Forming free-flowing pieces
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23P—SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
    • A23P10/00—Shaping or working of foodstuffs characterised by the products
    • A23P10/40—Shaping or working of foodstuffs characterised by the products free-flowing powder or instant powder, i.e. powder which is reconstituted rapidly when liquid is added
    • A23P10/47—Shaping or working of foodstuffs characterised by the products free-flowing powder or instant powder, i.e. powder which is reconstituted rapidly when liquid is added using additives, e.g. emulsifiers, wetting agents or dust-binding agents

Definitions

  • Encapsulated active compound powders have extensive use across a variety of industries, including food, beverages, cosmetics, and nutraceuticals.
  • the encapsulation provides a barrier against, for example, oxygen, light, and free radicals (Desai et al., Journal of Microencapsulation, 22(2), 179-192 (2005)).
  • Active compound powders typically are produced using a spray drying system.
  • such systems require high inlet and outlet temperatures, which can risk degrading the active compound or other components of the powder (Anwar et al., Journal of Food Engineering, 105, 367-378 (201 1)).
  • an active compound powder that is shelf stable, has improved loading capacity, and/or improved encapsulation efficiency.
  • the invention provides a method of providing an active compound powder comprising electrostatic spray drying a formulation comprising at least one active compound, an encapsulating agent, and optionally an excipient, at an inlet temperature of 150 °C or below and an exhaust temperature of 100 °C or below, wherein electrical charge is applied externally to droplets of active compound formulation feedstock liquid [claim 1], [0005]
  • the invention also provides a method of providing an oil emulsion powder comprising electrostatic spray drying an emulsion comprising at least one oil, an encapsulating agent, and optionally an emulsifier at an inlet temperature of 150 °C or below and an exhaust temperature of 100 °C or below, wherein electrical charge is applied externally to droplets of oil emulsion feedstock liquid [claim 2],
  • FIG. 1 is a vertical section of an illustrated spray dry ing system for processing an active compound containing-formulation into powder form according to an embodiment of the invention.
  • FIG. 2 is an enlarged vertical section of the electrostatic spray nozzle assembly of the illustrated spray drying system.
  • FIG. 3 A is a first cross-section view of an electrostatic spray nozzle assembly in accordance with an illustrative example
  • FIG. 3B is a second cross-section view of an electrostatic spray nozzle assembly in accordance with an illustrative example
  • FIG. 4 is a detail cross-section view of nozzle head section, including an induction ring, of the electrostatic spray nozzle assembly depicted in FIGs. 3A and 3B;
  • FIG. 5 is an exploded perspective view of the electrostatic spray nozzle assembly depicted in FIGs. 3A and 3B;
  • FIG. 6 shows the scanning electron micro (SEM) images of 20%, 50%, and 80% (w/w) vegetable oil load powders encapsulated by electrostatic spray dried (ESD) and spray dried (SD) at 5,000* magnification.
  • FIGs. 7A and 7B are SEM images of 50% and 80% (w/w) ESD powders comprising either coconut oil and medium-chain-triglycerides (MCT) from coconut (FIG. 4A) or flaxseed oil and olive oil (FIG. 4B), each at 5,000* magnification.
  • MCT medium-chain-triglycerides
  • FIG. 8 shows the SEM images of oil encapsulated powders containing 50% and 80% (w/w) fish oil and ghee at 5,000* magnification.
  • FIG. 9 shows the SEM images of oil encapsulated powders containing 50% (w/w) of either orange oil or mint oil, each at 5,000* magnification.
  • FIG. 10 shows the bacteria counts (log cfu/g, at 1% starter culture addition) for S. thermophilus (ST) and /.. bulgaricus (LB) at day 0 and after storage at 4 °C for 90 days.
  • FIG. 11 shows the SEM images of encapsulated oil-bacteria powders at 10,000* magnification.
  • FIG. 12 shows the SEM images of 40% oil load DHA oil powders prepared by conventional spray drying (CSD) and electrostatic spray drying (ESD) with different encapsulants: (i) maltodextrin and casein, (ii) maltodextrin and methylcellulose, and (hi) maltodextrin and saponin.
  • FIG. 13 shows the relationship between percentage of viable bacterial cells in a dried powder versus time (in days), after drying with: an electrostatic spray dryer with an internal negative charge system (Run 001), an electrostatic spray dry er with an external positive charge system (Run 032), and conventional freeze drying.
  • the present invention is predicated, at least in part, on the surprising discovery' that active compound powders that are spray dried using a traditional high heat spray drying system compared to a low heat, electrostatic spray system are limited in their loading capacity and/or encapsulation efficiency.
  • the invention provides a method of providing an active compound powder comprising electrostatic spray drying a formulation comprising at least one active compound, an encapsulating agent, and optionally an excipient, at an inlet temperature of 150 °C or below and an exhaust temperature of 100 °C or below.
  • the produced active compound powder has at least one benefit over a corresponding active compound powder produce by spray drying, such as being more shelf stable, improved loading capacity, and/or improved encapsulation efficiency, compared to a comparable active compound powder prepared using spray drying.
  • the invention also provides a method of providing an oil emulsion powder comprising electrostatic spray drying an emulsion comprising at least one oil, an encapsulating agent, and optionally an emulsifier at an inlet temperature of 150 °C or below and an exhaust temperature of 100 °C or below.
  • the inlet temperature is any suitable temperature that provides an active compound powder with the features described herein.
  • the inlet temperature is 150 °C or below (e.g., about 140 °C or below, about 135 °C or below, about 130 °C or below, about 125 °C or below, about 120 °C or below, about 115 °C or below, about 110 °C or below, about 105 °C or below, about 100 °C or below, about 95 °C or below, or about 90 °C or below).
  • the inlet temperature is about 140 °C or below, about 100 °C or below, about 150 °C, about 140 °C, or about 90 °C.
  • conventional spray drying systems have a much higher inlet temperature, typically about 140 °C or higher, e.g., 180-250 °C
  • the outlet temperature is any suitable temperature that provides an active compound powder with the features described herein.
  • the outlet temperature is about 80 °C or below (e.g., about 75 °C or below, about 70 °C or below, about 65 °C or below, about 60 °C or below, about 55 °C or below, about 50 °C or below, about 45 °C or below, about 40 °C or below, about 35 °C or below).
  • the outlet temperature is about 60 °C or below, about 50 °C or below, about 60 °C, about 50 °C, or about 35 °C.
  • conventional spray drying systems have outlet temperatures that are above 60 °C, typically about 95 °C.
  • the atomizing temperature of the electrostatic spray drying system also is relatively low, such as about 100 °C or below (e.g., about 95 °C or below, about 90 °C or below, about 85 °C or below, about 80 °C or below, about 75 °C or below, about 70 °C or below, about 65 °C or below, about 60 °C or below, about 55 °C or below, about 50 °C or below, about 45 °C or below, about 40 °C or below, about 35 °C or below, or about 30 °C or below).
  • about 100 °C or below e.g., about 95 °C or below, about 90 °C or below, about 85 °C or below, about 80 °C or below, about 75 °C or below, about 70 °C or below, about 65 °C or below, about 60 °C or below, about 55 °C or below, about 50 °C or below, about 45 °C or below, about 40 °C or
  • the electrostatic spray drying process applies a voltage to the spray droplets, which typically is about 0.1 kV or more (e.g., about 0.5 kV or more, about 1 kV or more, about 2 kV or more, about 4 kV or more, about 5 kV or more, about 7 kV or more, about 9 kV or more, about 12 kV or more, or about 15 kV or more).
  • the upper limit of the applied voltage typically is 30 kV and in some instances, the upper limit is 20 kV or more preferably 15 kV. Any two of the foregoing endpoints can be used to define a close- ended range, or a single endpoint can be used to define an open-ended range.
  • the applied voltage can be either continuous or modulated between two or more different voltages, known as Pulsed Width Modulation (PWM). Any two or more applied voltages ranging between 0.1-30 kV (e g., 0.5 kV and 1 kV, 1 kV and 5 kV, 1 kV and 10 kV, 5 kV and 15 kV) can be used for PWM to provide a desired effect, such as a particular agglomerate size.
  • the applied voltage is continuous.
  • the applied voltage is modulated between two or more different voltages, e.g., alternating between 1 kV and 10 kV.
  • the charge (positive or negative) of the applied voltage can be altered, as necessary.
  • altering the electrostatic charge can change the surface composition of the particle, the agglomeration properties and/or other physical properties of the particles produced.
  • an applied negative charge will allow more conductive compounds to move towards the surface of the particle and non-conductive compounds will remain near the core of the particle.
  • a negative electrostatic charge typically is applied in the electrostatic spray dry process when the charge is applied to the fluid internally with respect to the spray nozzle assembly disclosed herein.
  • a positive electrostatic charge typically is applied in the electrostatic spray dry process when the charge is applied to the fluid externally with respect to the spray nozzle assembly disclosed herein.
  • alternating the charge of the applied voltage is used when preparing an oil powder.
  • the oil to be used in the method is any suitable oil that can be subjected to the electrostatic spray dry process.
  • the at least one oil is plant or animal in origin.
  • the oil is an edible oil.
  • the oil can be provided by any source, including purchased commercially or extracted from a suitable plant (including a leaf, stem, root, nut, or seed) or animal source. Extraction can be by any suitable method, such as chemical solvent extraction and/or pressing.
  • oils examples include vegetable oil, vegetable shortening, castor oil, rice brain oil, olive oil, canola oil, com oil, palm oil, coconut oil, flaxseed oil, hempseed oil, rapeseed oil, linseed oil, grapeseed oil, rosehip seed oil, pomegranate seed oil, watermelon seed oil, seabuckthorn berry oil, camellia seed oil (tea oil), cranberry seed oil, hemp seed oil, borage seed oil, evening primrose oil, argan oil, jojoba oil, marula oil, carrot oil, sesame seed oil, sunflower oil, shea nut oil, soybean oil, peanut oil, walnut oil, almond oil, hazelnut oil, kukui nut oil, pecan oil, macadamia nut oil, meadowfoam oil, avocado oil, apricot kernel oil, an essential oil, silicone oil, fish oil, cocoa butter, shea butter, butter, ghee, medium chain triglycercides
  • an essential oil examples include, for example, aniseed oil, basil oil, bay oil, bergamot oil, cinnamon oil, clove oil, lavender oil, eucalyptus oil, lavender oil, ginger oil, geranium oil, rose oil, blue tansy oil, tea tree oil, moringa oil, lemon balm essential oil, lemongrass oil, thyme oil, rosemary oil, mint oil, lemon oil, orange oil, grapefruit oil, and fennel oil.
  • the encapsulating agent is any agent capable of encapsulating the active compound.
  • the encapsulating agent is a carbohydrate, a lipid, a protein, ascorbic acid, or a combination thereof.
  • the carbohydrate can be, e.g., maltodextrin, sucrose, dextrose, glucose, lactose, trehalose, amylase, cyclodextrin, dextrin, galactomannan, pectin, starch (e.g., com starch, waxy maize starch, native tapioca starch, pea starch), modified food starch (e.g., modified tapioca starch, OSA (octenyl succinic anhydride) modified starch), inulin, gum Arabic, guar gum, gellan gum, mesquite gum, xanthan gum, alginate, chitosan, shellac, carboxymethylcellulose, or a combination thereof.
  • starch e.g., com starch, waxy maize starch, native tapioca starch, pea starch
  • modified food starch e.g., modified tapioca starch, OSA (octenyl succ
  • Maltodextrins are usually classified by their dextrose equivalent value (DE) that range from 1 to 20. Maltodextrins with DE values of 4, 6, 10, 12, 15, 19, 20, 25, 30, and 42 are commerciallv available. Sources of maltodextrin include, e.g., maize, tapioca, and rice.
  • DE dextrose equivalent value
  • the lipid can be, e.g., a fatty acid or an ester thereof, a fatty' alcohol or an ester thereof, a triglyceride, a phospholipid, a glycolipid, an aminolipid, a lipopeptide, partial acylglycerol, or a combination thereof.
  • a suitable lipid examples include, e.g., carnauba wax, candelilla wax, beeswax, solid paraffin, rice bran wax, hydrogenated soybean oil, hydrogenated palm oil, palmitic acid, stearic acid, behenic acid, lauric acid, glyceryl tripalmitate glyceryl trimyristate, glyceryl trilaurate, cetyl alcohol, lauryl alcohol, stearyl alcohol, oleyl alcohol, and lecithin.
  • carnauba wax candelilla wax, beeswax, solid paraffin, rice bran wax, hydrogenated soybean oil, hydrogenated palm oil, palmitic acid, stearic acid, behenic acid, lauric acid, glyceryl tripalmitate glyceryl trimyristate, glyceryl trilaurate, cetyl alcohol, lauryl alcohol, stearyl alcohol, oleyl alcohol, and lecithin.
  • the protein can be protein from a plant source or an animal source (e g , milk).
  • proteins include, e.g., casein, a caseinate (e g., sodium caseinate, calcium caseinate, calcium phosphate caseinate), gelatin, casein, soy protein, wheat protein, whey protein, rice protein, pea protein, cocoa shell protein, or a combination thereof.
  • the processing conditions provide an emulsion between the at least one oil and encapsulating agent.
  • the emulsion comprises an emulsifier.
  • the emulsifier is any suitable surfactant that enables the production of an emulsified powder between the oil and the encapsulating agent.
  • One or more than one (e.g., 2, 3, 4, etc.) emulsifiers can be used in the composition.
  • the emulsifier is at least one selected from casein, a caseinate (e g., sodium caseinate, calcium caseinate, calcium phosphate caseinate), lecithin, saponin (e.g., quilaja, glycyrrhizic acid), carrageenan, gum Arabic (GA), xanthan, whey protein isolate (WPI), whey protein concentrate (WPC), stearate, glyceryl monostearate, sucrose ester, monopropylene glycol, propylene glycol ester of fatty acid, poly glycerol esters of fatty acid, a mono- and diglycerol, mono- and digly cerides of fatty acids (e.g., citric acid ester of monoglyceride (CAEM), saturated distilled monoglyceride (SDM), polyglycerol fatty acid ester (PGFE), succinylated monoglyceride (SMG), lecithin (LC)), distilled monoglyceride,
  • the formulation comprises at least one active compound that is part of the powder product.
  • One active compound or more than one active compound e.g., 2, 3, 4, 5, etc.
  • Typical active compounds include, e.g., an antioxidant, a vitamin, a bacterium, an omega oil, an essential oil, a flavoring agent, a pigment, a dye, and a combination thereof.
  • an antioxidant can be used to inhibit oxidation and help stabilize the active compound, particularly an oil.
  • Suitable antioxidants include, for example, butylated hydroxy anisole (BHA), butylated hydroxytoluene (BHT), propyl gallate (PG), tert-butyl hydroquinone (TBHQ), [3-carotene, ascorbic acid, tocopherol, tea extract, rosemary extract, sage extract, thyme extract, alkannin, shikonin, ascorbyl palmitate, and a flavonoid (e.g., catechin, apicatechins, epicatechin gallate, epigallocatechin, and epigallocatechin gallate).
  • BHA butylated hydroxy anisole
  • BHT butylated hydroxytoluene
  • PG propyl gallate
  • TBHQ tert-butyl hydroquinone
  • [3-carotene ascorbic acid, tocopherol, tea extract, rosemary extract, sage extract, thyme extract, alkannin, shikonin, ascor
  • Vitamins include, for example, vitamin A, B, C, D, E, and K, including the vitamers of each thereof.
  • the bacterium includes, for example, a starter culture, a probiotic, and a combination thereof.
  • the starter culture can be, for example, from the genus lactobacillus, streptococcus, and leuconostoc.
  • Specific examples of a starter culture include, e.g., L. bulgaricus, L. lactis, L. acidophilus, L. helveticus, L. casei. L. plantarum, L. rhamnosus, Leuconostoc citrovorum, Leuconostoc dextranicum, S. lactis, S. cremoris, S. diacetylactis, S. durans, S. faecalis, S.
  • thermophilus propionic bacterium shermanii, and combinations thereof.
  • Suitable probiotics include those from the genus bifidobacteria, lactobacillus, and saccharomyces , preferably bifidobacteria or lactobacillus.
  • Specific examples of probiotic include, e.g., B. animalis, B. breve, B. lactis, B. longum, L. acidophilus, L. reuteri, S. bourladii, and combinations thereof.
  • the omega oil also known as an omega-3 oil, is a polyunsaturated fatty acid with a double bond three atoms away from the terminal methyl group. Examples include, eicosapentaenoic acid (EP A), docosahexaenoic acid (DHA), a-linolenic acid (ALA), and a combination thereof.
  • EP A eicosapentaenoic acid
  • DHA docosahexaenoic acid
  • ALA a-linolenic acid
  • the essential oil as an active compound is as described herein.
  • the flavoring agent can be in the form of an oil, a non-aqueous solution, or an emulsion.
  • the flavoring agent can be natural or synthetic. Suitable examples include, e.g., limonene, fenchone, vanillin, thymol, menthol, isoamyl acetate, benzaldehyde, ethyl propionate, ethyl butyrate, methyl anthranilate, methyl salicylate, ethyl decadienoate, allyl hexanoate, ethyl maltol, 2,4-dithiapentance, fumaric acid, acetic acid, ascorbic acid, citric acid, lactic acid, malic acid, phosphoric acid, tartaric acid, citral, massoia lactone, acetoin, manzanate, cinnamaldehyde, a glutamate (e.g., mono- and/or disodium
  • the pigment or dye can be natural or synthetic and include, for example, a mineral, a clay, charcoal, carbon black, ultramarine, ultramarine green shade, Tyrian red, Indian yellow, a cadmium-based pigment (e.g., cadmium yellow, cadmium ted, cadmium green, cadmium orange), a chromium-based pigment (e.g., chrome yellow, chrome green), a cobalt-based pigment (e.g., cobalt violet, cobalt blue, cerulean blue, aureolin), a copper-based pigment (e.g., azurite, Han purple, Han blue, an Egyptian blue,, malachite, Paris green, phthalocyanine blue BN, phthalocyanine Green G, verdigris), iron oxidebased pigment (e.g., sanguine, caput mortuum, oxide red, red ochre, yellow ochre, Venetian red, Prussian blue), a lead-based pigment (e.g.
  • Direct Black 171 sunset yellow, tartrazine, azorubine, ponceau, amaranth, allura red
  • an acid dye e.g., Indian ink, congo red, nigrosoine
  • a naphthol an azoic
  • a nitro dye e.g., maritus yellow
  • an anthraquinone dye e.g., C.I. Reactive Blue 19, indanthrone, alizarin, 1- aminoanthraquinone
  • a sulfur dye e.g., indophenol, sulfur black, sulfur red 7
  • turmeric and combinations thereof.
  • the oil emulsion powder produced by the method has a lower amount of surface free fat, i.e., oil, compared to a spray dried powder of the same oil emulsion.
  • the oil powder product can have 40% surface free fat or less (e.g., 37% or less, 35% or less, 30% or less, 25% or less, 20% or less, 10% or less, 8% or less, 6% or less, 5% or less, 4% or less, 3% or less, 2% or less, 1% or less, 0.5% or less, or 0.2% or less).
  • the percentage of surface free fat or oil can be determined as follows:
  • the oil emulsion powder has any suitable oil load (e.g., about 1-90%).
  • the oil load can be about 1% or more (e.g., about 5% or more, about 10% or more, about 15% or more, about 20% or more, about 25% or more, about 30% or more, about 35% or more, about 40% or more, about 45% or more, about 50% or more, about 55% or more, about 60% or more, about 65% or more, about 70% or more, about 75% or more, about 80% or more, or about 85% or more).
  • the upper limit of the oil load is typically about 90% or less (e.g., about 85% or less, about 80% or less, about 75% or less, about 70% or less, about 65% or less, about 60% or less, about 55% or less, about 50% or less, about 45% or less, about 40% or less, about 35% or less, about 30% or less, about 25% or less, about 20% or less, about 15% or less, or about 10% or less). Any two of the foregoing endpoints can be used to define a close-ended range, or a single endpoint can be used to define an open-ended range. Tn an aspect, the oil powder produced by the claimed method has a higher oil load (e.g., 20% or more, 50% or more, 60% or more, 70% or more, or 80% or more, about 90%).
  • a higher oil load e.g. 20% or more, 50% or more, 60% or more, 70% or more, or 80% or more, about 90%).
  • the active compound formulated powder has an encapsulation efficiency of 50% or more (e.g., 55% or more, 60% or more, 65% or more, 70% or more, 75% or more, 80% or more, 85% or more, 90% or more, 92% or more, 95% or more, 96% or more, 97% or more, 98% or more, and 99% or more).
  • Active encapsulation efficiency can be determined as follows:
  • the method provides an improved oil load and encapsulation efficiency compared to a spray dried powder of the same oil emulsion.
  • the oil load of the produced oil powder can range from 1-60% in combination with an encapsulation efficiency that ranges from 90-99%.
  • the oil load can range from 61-90% in combination with an encapsulation efficiency that ranges from 55-90%.
  • the active compound powder product has a low moisture content, typically about 5% or less (e.g., about 4.5% or less, about 4% or less, about 3.5% or less, about 3% or less, about 2.5% or less, about 2% or less), preferably in combination with a low water activity (e.g., about 0.3 or less, including about 0.28 or less, about 0.25 or less, about 0.2 or less, about 0. 18 or less, about 0.15 or less, or about 0. 1 or less).
  • the active compound powder product has a moisture content of about 4% or less or about 3% or less.
  • FIG. 1 is an illustrated spray drying system 10 for processing an active compound encapsulation formulation into powder form according to the invention.
  • a basic construction and operation of the illustrated spray drying system 10 is similar to that disclosed in U.S. Patent 10,286,411, assigned to the same assignee as the present application, the disclosure of which is incorporated herein by reference.
  • the spray dry ing system 10 in this case includes a processing tower 11 comprising a drying chamber 12 in the form of an upstanding cylindrical structure, a top closure arrangement in the form of a cover or lid 14 for the drying chamber 12 having a heating air inlet 15 and a liquid spray nozzle assembly 16, and a bottom closure arrangement in the form of a powder collection cone 18 supported at the bottom of the drying chamber 12, a filter element housing 19 through which the powder collection cone 18 extends having a heating air exhaust outlet, and a bottom powder collection chamber 21.
  • a processing tower 11 comprising a drying chamber 12 in the form of an upstanding cylindrical structure, a top closure arrangement in the form of a cover or lid 14 for the drying chamber 12 having a heating air inlet 15 and a liquid spray nozzle assembly 16, and a bottom closure arrangement in the form of a powder collection cone 18 supported at the bottom of the drying chamber 12, a filter element housing 19 through which the powder collection cone 18 extends having a heating air exhaust outlet, and a bottom powder collection chamber 21.
  • the illustrated drying chamber 12 has a “replaceable internal non-metallic” insulating liner 22 disposed in concentric spaced relation to the inside wall surface 12a of the drying chamber 12 into which electrostatically charged liquid spray particles from the spray nozzle assembly 1 are discharged.
  • the liner 100 has a diameter d less than the internal diameter dl of the drying chamber 12 so as to provide an insulating air spacing 101 with the inner wall surface 12a of the drying chamber 12.
  • the liner 100 preferably is non-structural being made of a non-permeable flexible plastic material.
  • the spray nozzle assembly 16 is a pressurized air assisted electrostatic spray nozzle assembly for directing a spray of electrostatically charged particles into the dryer chamber 12 for quick and efficient drying of an active compound encapsulated formulation into powder form.
  • the illustrated spray nozzle assembly 16 includes a nozzle supporting head 31, an elongated nozzle barrel or body 32 extending downstream from the head 31, and a discharge spray tip assembly 34 at a downstream end of the elongated nozzle body 32.
  • the head 31 in this case is made of plastic or other non-conductive material and formed with a radial liquid inlet passage 36 that receives and communicates with a liquid mlet fitting 38 for coupling to a supply line 37 that communicates with a supply of an active compound powder product to be spray dried
  • the nozzle supporting head 31 in this case further is formed with a radial pressurized air atomizing inlet passage 39 downstream of said liquid inlet passage 36 that receives and communicates with an air inlet fitting 40 coupled to a suitable pressurized gas supply.
  • the head 31 also has a radial passage 41 upstream of the liquid inlet passage 36 that receives a fitting 42 for securing a high voltage cable 44 connected to a high voltage source and having an end 44a extending into the passage 41 in abutting electrically contacting relation to an electrode 48 axially supported within the head 31 and extending downstream of the liquid inlet passage 36.
  • the electrode 48 is formed with an internal axial passage 49 communicating with the liquid inlet passage 36 and extending downstream though the electrode 48.
  • the electrode 48 is formed with a plurality of radial passages 50 communicating between the liquid inlet passage 36 and the internal axial passage 49.
  • the elongated body 32 is in the form of an outer cylindrical body member 55 made of plastic or other suitable nonconductive material, having an upstream end 55a threadably engaged within a threaded bore of the head 31.
  • the liquid feed tube 58 is disposed in electrical contacting relation with the electrode 48 for efficiently electrically charging liquid throughout its passage from the head 31 and through elongated nozzle body member 32 to the discharge spray tip assembly 34, which in this case is similar to that disclosed in U.S. Patent 10,286,411.
  • fluid is charged internally with respect to the spray nozzle assembly 1 . More specifically, the fluid is charged as it passes through the liquid feed tube 58 prior to the fluid exiting the spray nozzle assembly 16.
  • FIGs. 3-5 A further embodiment of a spray nozzle assembly 130 for use in the spraying drying system 10 of FIG. 1 is shown in FIGs. 3-5.
  • the spray nozzle 130 is specially configured nozzle assembly that, in operation, exhibits certain electrical properties facilitating generation of a continuous flow of electrostatically charged spray droplets.
  • FIG. 3A an exemplary electrostatic spray nozzle arrangement is illustratively depicted where electrostatic charging of spray droplets is achieved by an electrical circuit arrangement including an induction ring 210 provided in the form of an electrically conductive metal retaining cap positioned at an exit aperture of the spray nozzle 130.
  • An opening 215 of the induction ring 210 is sufficiently wide to avoid, with the aid of a purging gas stream, excessive buildup of the active compound formulation emitted from an opening of an atomizing gas cap 220 that passes in droplet form through the opening 215.
  • the opening 215 has an inner diameter on the order of less than 1 inch for an applied electrical field having a voltage of 3,000 to 4,000 volts (3-4 kilovolts). More particularly, the opening 215 has a diameter of about 0.7 inches.
  • the diameter of the opening 215 and/or the applied voltage are modified in accordance with spray pattern (wide/narrow spray field), nozzle aperture position (linear displacement along path of spray field) in relation to the opening 215 of the induction ring 210.
  • the atomizing gas cap 220 is anon-conductive insulating material (e.g., a rigid plastic material).
  • a first conductive path is provided for generating an electrostatic field at the opening 215 of the induction ring 210 to electrostatically charge droplets of active compound formulation emitted from the atomizing gas cap.
  • the induction ring 210 physically (by complementary screw threating) and conductively engages an electrically conductive surface of a nozzle head 230.
  • the first conductive path is further provided by a further physical and conductive engagement of the nozzle head 230 with a purge gas tube 240.
  • the nozzle head 230 and the purge gas tube 240 are physically and conductively engaged by complementary screw thread surfaces at 242.
  • the purge gas tube 240 is also provided with an electrically conductive surface providing an electrically conductive path from the nozzle head 230 to an induction field (high voltage) electrode 250 from a high voltage field signal source (not shown).
  • outer surfaces of electrically conductive components are coated with an electrically insulating layer to reduce the possibility of arcing within the spraying environment.
  • an electrically insulating layer is provided by, for example, a polytetrafluoroethylene (PTFE) coating.
  • all exposed surfaces of electrically conductive components - even the inner exposed surface of the induction ring 210 - are coated with a strong dielectric material (e.g. PTFE) to provide an electrical insulating barrier between the high (magnitude) voltage of the induction ring 210 and low (magnitude) voltage of the active compound formulation as well as any potentially ground connection sources to which the feed stock comes into contact prior to exiting the spray nozzle.
  • a strong dielectric material e.g. PTFE
  • Such arrangement facilitates preventing, minimizing any current flow from the induction ring during operation of the illustrative electrostatic spray drying system.
  • a second conductive path is provided for establishing a complementary electrical (e.g.
  • the second conductive path provides a source for inducing a charge (opposite the field potential generated at the opening 215) on the droplets passing from a fluid tip 280 having an electrically grounded conductive surface in contact with the active compound formulation through an electric field at the opening 215.
  • the second conductive path continues at a physical and electrical connection between the fluid tip 280 and a fluid tube 285 that provides the feedstock to the fluid tip 280.
  • an electrically insulating layer e.g., PTFE
  • An atomizing gas tube 290 provides atomizing gas to the atomizing gas cap 220.
  • the atomizing gas tube 290 is, by way of example made of a non-electrically conductive material (e.g. a rigid plastic, ceramic, etc.) that is configured to provide a sealed engagement with the atomizing gas cap 220.
  • the atomizing gas tube 290 comprises a conductive material coated with an electrically insulating material.
  • the atomizing gas tube 290 and atomizing gas cap 220 provide an electrically insulating barrier between the first conductive path and the second conductive path described herein above. It is noted that such electrically insulating characteristic may alternatively be achieved by coating exposed surfaces with an insulating coating (e.g. PTFE).
  • a nozzle body 260 is physically configured with several receptacles/openings for maintaining physical/electrical engagement between components of the spray nozzle 130 illustratively depicted herein.
  • the nozzle body 260 includes an induction field electrode receptacle 255 holding the induction field electrode 250 in electrically conductive engagement with the electrically conductive surface of the purge gas tube 240.
  • the nozzle body 260 includes a ground electrode receptacle 270 holding an electrical ground electrode 275 in electrically conductive engagement with the electrically conductive surface of the fluid tube 285.
  • An induction ring purge gas port 277 provides an opening for feeding a purge gas that flows through the purge gas tube 240 to the opening 215 in the induction ring 210.
  • the nozzle body 260 further includes an atomizing gas port 295 that provides an opening for feeding an atomizing gas to the atomizing gas tube 290.
  • the nozzle body 260 includes a cylindrical receptacle having a threaded surface at 265 to hold in place the purge gas tube 240 having a complementary' threaded outer surface.
  • FIG. 4 an additional detailed view is provided of the nozzle head portion of the spray nozzle depicted in FIGs. 3A and 3B to enable a clearer view of the various physical relationships depicted in FIGs. 3A and 3B and the corresponding written description provided herein above.
  • FIG. 5 provides an exploded perspective view of the electrostatic spray nozzle assembly depicted in FIGs. 3A and 3B to provide additional visual details of the illustrative example of an electrostatic spray nozzle in accordance with the current disclosure.
  • the spray nozzle assembly 130 of FIGs. 3-5 charges the fluid (via the induction ring 210) after it exits the spray nozzle assembly in droplet form.
  • This external charge configuration can offer several advantages over the internal charge arrangement of FIG. 2 including the ability to use significantly lower voltages which can lead, among other things, to increased safety. Further, the external charge arrangement can have cost advantages by eliminating the need for special electrically insulated components along the liquid feed path.
  • the electrostatic spray drying system 10 is operable for drying active compound powders into fine particles with improved characteristics over the prior art.
  • the term “about” typically refers to ⁇ 1% of a value, ⁇ 5% of a value, or ⁇ 10% of a value.
  • a method of providing an active compound powder comprising electrostatic spray drying a formulation comprising at least one active compound, an encapsulating agent, and optionally an excipient at an inlet temperature of 150 °C or below and an exhaust temperature of 100 °C or below, wherein electrical charge is applied externally to droplets of active compound formulation feedstock liquid.
  • a method of providing an oil emulsion powder comprising electrostatic spray drying an emulsion comprising at least one oil, an encapsulating agent, and optionally an emulsifier at an inlet temperature of 150 °C or below and an exhaust temperature of 100 °C or below, wherein electrical charge is applied externally to droplets of oil emulsion feedstock liquid.
  • the at least one oil is vegetable oil, vegetable shortening, castor oil, rice brain oil, olive oil, canola oil, com oil, palm oil, coconut oil, flaxseed oil, hempseed oil, rapeseed oil, linseed oil, grapeseed oil, rosehip seed oil, pomegranate seed oil, watermelon seed oil, seabuckthorn berry oil, camellia seed oil (tea oil), cranberry seed oil, hemp seed oil, borage seed oil, evening primrose oil, argan oil, jojoba oil, marula oil, carrot oil, sesame seed oil, sunflower oil, shea nut oil, soybean oil, peanut oil, walnut oil, almond oil, hazelnut oil, kukui nut oil, pecan oil, macadamia nut oil, meadowfoam oil, avocado oil, apricot kernel oil, an essential oil, silicone oil, fish oil, cocoa butter, shea butter, butter, ghee
  • the lipid is a fatty acid or an ester thereof, a fatty alcohol or an ester thereof, a triglyceride, a phospholipid, a glycolipid, an aminolipid, a lipopeptide, partial acylglycerol, or a combination thereof.
  • the protein is casein, caseinate, gelatin, soy protein, wheat protein, whey protein, rice protein, pea protein, cocoa shell protein, or a combination thereof.
  • the emulsifier is at least one selected from casein, caseinate, lecithin, saponin, carrageenan, gum Arabic, xanthan, whey protein isolate, stearate, glyceryl monostearate, sucrose ester, monopropylene glycol, propylene glycol ester of fatty' acid, poly glycerol esters of fatty' acid, a mono- and diglycerol, mono- and diglycerides of fatty acids, distilled monoglyceride, poly glycerol polyricinoleate, polysorbate 80, a sorbitan ester, a lactylated ester, an ethoxylated ester, a succinated ester, a fruit acid ester, carboxymethyl cellulose, and a combination thereof.
  • This example demonstrates low temperature electrostatic spray drying of an oil powder product in an embodiment of the invention.
  • Oil emulsion powders were made by electrostatic spray drying (ESD) at inlet temperatures of 90 °C, 140 °C, and 150 °C, however, the inlet drying temperature can be as low as 80 °C.
  • Atomizing temperature was generally maintained below 80 °C and the exhaust temperature below 60 °C. In this example, the atomizing temperature was set to 35 °C, 50 °C, and 80 °C to obtain exhaust temperatures of 35 °C, 50 °C, and 60 °C, respectively.
  • Negative pulsed width modulation (PWM) alternating between lOkV and IkV was used in these examples, however, electrostatic charge may be positive, and it may be as low as 0.
  • PWM pulsed width modulation
  • Atomizing gas pressure may range from 30-552kPa.
  • oil emulsion powders were also spray dried at 180 °C inlet and 90 °C exhaust by conventional high heat spray drying. The processing parameters are shown in Table 1.
  • This example demonstrates low temperature electrostatic spray drying of a vegetable oil powder product in an embodiment of the invention.
  • Vegetable oil emulsions were formulated to contain 20% to 90% (w/w) vegetable oil, encapsulated with maltodextrin and stabilized with sodium caseinate. Oil emulsions were spray dried (SD) at 180 °C and electrostatic spray dried (ESD) with 10 kV PWM at 90 °C and 140 °C. Table 2 shows the moisture content and water activity of the resulting vegetable oil powders. Moisture content was below 3% in all powders and water activity below 0.22.
  • Table 3 shows the oil load, surface free fat, encapsulation efficiency, and peroxide value of vegetable oil powders
  • the peroxide values (in all of the examples except Example 7) were measured soon after preparation of the powders using the spectrophotometric standard method of the International Dairy Federation (IDF) (see, e.g., Rahmani-Manglano et al., Foods, 9, 545, 21 pages (2020)).
  • IDF International Dairy Federation
  • Electrostatic spray drying produced powders with greater encapsulation efficiency than spray drying at 20%, 50%, and 80% oil load. Overall, the encapsulation efficiency drops with increasing oil load. At 20% oil load, the encapsulation efficiency was greater than 99% in ESD powders and lower than 97% in spray dried powders. At 50% oil load, the encapsulation efficiency was more than 97% in ESD powders compared to less than 90% in spray dried powders. At 80% oil load, ESD powders had 73% encapsulation efficiency compared to 53% by spray drying.
  • FIG. 6 shows the scanning electron micro (SEM) images of 20%, 50%, and 80% (w/w) vegetable oil load powders encapsulated by electrostatic spray dried (ESD) and spray dried (SD) at 5,000x magnification.
  • ESD electrostatic spray dried
  • SD spray dried
  • This example demonstrates low temperature electrostatic spray drying of a plant-based oil powder product in an embodiment of the invention.
  • coconut oil, medium-chain-triglycerides (MCT) from coconut, flaxseed oil and olive oil emulsions were formulated to contain 50% and 80% (w/w) oil, encapsulated with maltodextrin and stabilized with sodium caseinate. Emulsions were then dried using electrostatic spray drying at temperatures of 90 °C mlet and 35 °C outlet.
  • MCT medium-chain-triglycerides
  • Table 4 shows the moisture content and water activity of resulting powders. All the powders had a moisture content below 4% and a water activity below 0.28. Moisture and water activity were higher in powders with greater oil load.
  • Table 5 shows the oil load, surface free fat, encapsulation efficiency and peroxide value of coconut oil, MCT, flaxseed oil, and olive oil powders.
  • the surface free fat was approximately 1-1.2% and this increased to 16-20% at 80% oil load in all powders.
  • Encapsulation efficiency was > 97% at 50% oil load and 74-79% in powders containing 80% oil.
  • FIGs. 7A and 7B show the SEM images of 50% and 80% oil load of different oil powders.
  • FIG. 7A shows coconut oil and MCT particles
  • FIG. 4B shows flaxseed oil and olive oil particles. Primary particles were similar in appearance for all oil types at an equivalent oil load. Differences were observed between 50% and 80% oil load powders, with primary particles in the 80% oil powders showing distinct spherical appearance.
  • This example demonstrates low temperature electrostatic spray drying of an animal-based oil powder product in an embodiment of the invention.
  • Table 6 shows the moisture content and water activity of the resulting powders. All powders had a moisture content below 3% and a water activity below 0.2 at 50% oil load and less than 0.25 at 80% oil load. Table 6.
  • Table 7 shows the oil load, surface free fat, encapsulation efficiency, and peroxide value of the fish oil and ghee powders. At 50% oil load, the surface free fat was approximately 1.1 -1.3% and this increased to 17-20% at 80% oil load in all powders.
  • the encapsulation efficiency was > 97% at 50% oil load and 74-78% in powders containing 80% oil.
  • FIG. 8 shows the SEM images of 50% and 80% oil load fish oil and ghee powders. The primary particles were similar in appearance for both oil types at an equivalent oil load. Differences were observed between 50% and 80% oil load powders, with primary particles in the 80% oil powders showing a distinct spherical appearance.
  • This example demonstrates low temperature electrostatic spray drying of an essential oil powder product in an embodiment of the invention.
  • Orange and mint oil emulsions were formulated to contain 50% (w/w) oil, encapsulated with maltodextrin and stabilized with sodium caseinate. Emulsions were then dried using electrostatic spray dry ing at temperatures of 90/35 °C and 150/60 °C inlet and outlet temperatures, respectively. Negative pulsed width modulation (PWM) alternating between l OkV and IkV was used in these examples.
  • PWM pulsed width modulation
  • Table 8 shows the water activity of resulting powders. All powders had water activity between 0.1 and 0.23.
  • Mint50%Oil 150/60 0.096 ⁇ 0.002 sd standard deviation
  • FIG. 9 shows the SEM images of 50% oil load orange and mint powders at two dry ing temperatures. The primary particles were similar in appearance for both oil types. Differences were observed between orange and mint oil powders, with primary particles in mint oil powders showing more distinct porous surfaces.
  • This example demonstrates low temperature electrostatic spray drying of an encapsulated oil-bacteria powder product in an embodiment of the invention.
  • Vegetable oil emulsions were formulated to contain 50% (w/w) oil and 1%, 10% or 20% (w/w) starter culture ( . thermophilus and L bulgaricus mixture).
  • Maltodextnn was the encapsulant, and the emulsion was stabilized with sodium caseinate. Emulsions were dried using electrostatic spray drying at 90 °C inlet and 35 °C outlet. Negative pulsed width modulation (PWM) alternating between lOkV and IkV was used in these examples.
  • PWM pulsed width modulation
  • All powders had a moisture content below 4% and water activity below 0.25 with 1 % and 10% starter culture addition. At 20% culture addition the water activity increase to 0.3.
  • Table 10 shows the oil load, surface free fat, encapsulation efficiency, and peroxide value for oil-bacteria powders. At 1%, 10%, and 20% culture addition, the surface free fat was less than 1% and the encapsulation efficiency was > 98%. The peroxide values were low ( ⁇ 0.2 meq Ch/kg oil).
  • FIG. 10 shows the bacteria counts (log cfu/g, at 1% starter culture addition) for S. thermophilus (ST) and L. bulgaricus (LB) at day 0 and after storage at 4 °C for 90 days.
  • the viability of S. thermophilus and L. bulgaricus remained higher (>7 log cfu/g for ST and >6 log cfu/g for LB) even after 90 days storage.
  • FIG. 11 shows the SEM images of the encapsulated oil-bacteria powders. The primary' particles were similar in appearance irrespective of the different loads of starter bacteria.
  • This example demonstrates low temperature electrostatic spray drying of a docosahexaenoic acid (DHA) oil powder product from microalgae in an embodiment of the invention.
  • DHA docosahexaenoic acid
  • DHA emulsions were formulated to contain 40% (w/w) oil, encapsulated using four different formulations: (i) modified starch, (ii) maltodextrin and casein, (iii) maltodextrin and methylcellulose, and (iv) maltodextrin and saponin (Quilaja).
  • Emulsions were dried using either conventional spray drying (CSD) at an inlet temperature of 120 °C, electrostatic spray drying (ESD) at an inlet temperature of 120 °C with negative voltage at 8 kV, or freeze drying (FD).
  • Table 12 shows the water activity and the encapsulation efficiency. All the powders had a water activity below 0.52, but the ESD powders had a water activity' below 0.23.
  • the peroxide values were measured after 2 months of storage of the resulting powders at 40 °C in the oven using the titration method established by the International Fragrance Association (IFRA) (see, e.g., IFRA Analytical Method, “Determination of the Peroxide Value,” September 10, 20219; and Kaya et al., Food Science and Technology, 141, 110872 (2021)).
  • IFRA International Fragrance Association
  • the encapsulation efficiency ranged between 19-100%.
  • the formulation impacted the encapsulation efficiency.
  • the peroxide values were between 143 to 1550 meq Ch/kg oil after 2 months at 40 °C in the dark.
  • FIG. 12 shows the SEM images of 40% oil load DHA oil CSD and ESD powders with the different formulations.
  • the primary particles were similar in appearance with the same size for all formulation. Differences were observed between the ESD and CSD powders, with a deflated balloon shape more pronounced for ESD than for CSD.
  • the deflated balloon is characteristic of low air inlet and outlet temperatures. This shape also is likely attributed to the fact that the elastic regime is quickly reached during the drying (see, e.g., Sadek et al., Food Hydrocolloids, 48, 8-16 (2015)).
  • EXAMPLE 8 [0133] This example compares powder products for encapsulation of oil using an electrostatic spray drying (ESD) system wherein the charge is applied externally to one wherein the charge is applied internally in an embodiment of the invention.
  • ESD electrostatic spray drying
  • the core material can comprise 5% to 90% by weight and the wall material can comprise 10% to 95% by weight of the feedstock solution, based on the total dry weight to the core material and the wall material combined.
  • the feedstock solution may have a viscosity of 1 mPa s to 10,000 mPa s, preferably 50 to 250 mPa s, and the solid content can be between 2 and 75%.
  • Table 13 shows a formulation of oil encapsulation feedstock used in the present example.
  • Capsul TA is a modified food starch derived from tapioca (Ingredion, Westchester, IL, USA) used as the encapsulation agent instead of maltodextrin. Capsul TA and water were mixed 12 hours before adding to oil, then the total mixture was homogenized for 30 min at 3600 RPM.
  • Table 14 shows set up of Fluid Air PolarDry® system Model 032 electrostatic spray dryer (Spraying Systems, Naperville, IL, USA) used in the example.
  • the system parameters are generally similar to those used for an ESD system with an internal charge, except that lower voltages can be applied.
  • a constant charge between 0. 1 kV and 0.5 kV, or a pulsed charge alternating between 0 and 5 kV, can be used with an atomizing gas to create droplets in an inert drying gas.
  • the charge can be positive or negative.
  • the pressure of the atomizing gas can be between 0.2 to 6 bars.
  • the inlet drying gas temperature can be between 40 to 150 °C.
  • the inert gas flowrate is between 2 to 20 000 Nm 3 /h.
  • Table 15 shows the operating parameters of the ESD used in the present example.
  • Table 16 shows the size distributions of the particles produced in runs la (internal charge) and lb (external charge), determined using a Malvern Panalytical MasterSizer 3000 instrument with an Aero S or Hydro EV accessory (Spectris pic, London, UK).
  • Runlb resulted in larger particle agglomerations at every point along the particle size distribution than Run la did.
  • Wettability i.e., capacity' of powder particles to absorb water on their surface
  • IDF (1979) Determination of the dispersibility and wettability of instant dned milk.” IDF Standard No. 87. International Dairy Federation, Brussels) and GEA Niro Method No. A 6 a (revised 2005).
  • Table 17 shows the moisture content of the powders produced in Runs la and lb, determined using a thermobalance (Sartorius MA37, Sartorius AG, Gottingen, Germany) at a temperature of 110°C with 1-2 g of sample powder.
  • the moisture content of the final powder has to be below 5%.
  • the maximum feed rate that results in a moisture content ⁇ 5% is 56 - 60 LPH, i.e., 56 - 60 kg/h.
  • the moisture content of Run la was 2.8 and that of Run lb was 2.23.
  • Table 18 shows the surface oil content and oil encapsulation efficiency of powders produced with the ESD spray dryer system having either internal or external charge nozzles, compared to the values for a powder produced by a conventional high temperature spray dryer, the Buchi B290 (Buchi, Switzerland).
  • the surface oil content of sample prepared with the ESD system was essentially the same with both the internal and external charge nozzles, and both values were greater than for the comparative Buchi spray dryer.
  • the oil encapsulation efficiency was substantially improved in the ESD system of the present invention, with the oil encapsulation efficiency being essentially 100% for the ESD system with the nozzle applying the charge externally.
  • This example compares encapsulated bacteria powder products prepared using an electrostatic spray drying (ESD) system wherein the charge is applied externally to one wherein the charge is applied internally in an embodiment of the invention.
  • ESD electrostatic spray drying
  • Table 19 shows a formulation of bacteria encapsulation feedstock used in the present example. Table 19.
  • This example used Lactobacillus Rhamnosus (LGG) from CHR Hanssen.
  • LGG Lactobacillus Rhamnosus
  • 1.4 g of LGG was added to a solution of maltodextrin DEI 9 (20% dry weight) (Glucidex® 19, Roquette). 400 g of solution was dried at laboratory scale for SD, FD and ESD. At industrial scale, the feedstock quantity was adjusted regarding evaporation capacities of each technology and expected yield.
  • Model 001 is a lab-scale spray dryer system
  • Model 032 is a larger, pilot-scale system.
  • Table 21 shows the operating conditions of Models 001 and 032 electrostatic spray dryers used in the example.
  • Table 22 shows the operating conditions of the Cryotec Pilote bench model (Saint-Gely-du-Fesc, France) freeze dryer used in the example.
  • Table 23 shows the water activity of the dried powders, determined using Rotronic equipment.
  • the bacteria powders were analysed for content of viable cells using the following method: 1 g of powder was resuspended in 10 mL of TS buffer; an appropriate serial dilution was made; and ImL of each final solution was placed onto an MRS agar plate. The percentage of cell survival was defined as the ratio between log (CFU/g) of viable cells, before and after drying. To assess stability over time, the same measurements were done at different time over 2 months.
  • FIG. 13 shows a graph depicting the relationship between percentage of viable bacterial cells in the dried powders versus time (in days), after drying with: electrostatic spray drying with an internal negative charge system (Run Model 001), with an external positive charge system (Run Model 032), and with conventional freeze drying.
  • the results show that the electrostatic spray dried powders exhibited similar stability to the freeze dried powder, and may be more stable after an extended time, i.e., around 2 months. Even though the outlet temperature was 10°C higher during the spray drying with the external charge in the Model 032 system, when compared to the conditions for spray drying with an internal charge in the Model 001 system, the oil-bacterial powders exhibited similar stability with time.
  • This example compares the effects of external vs. internal applied charge and different inlet temperature on the encapsulation efficiency of volatile oil (Peppermint oil) in an embodiment of the invention.
  • Table 24 shows a formulation of oil Peppermint oil encapsulation feedstock used in the present example.
  • Capsul TA was hydrated overnight, then combined with the peppermint oil and homogenized for 30 min.
  • Table 25 shows set up of Fluid Air PolarDry® system Model 032 electrostatic spray dryer (Spraying Systems, Naperville, IL, USA) used all runs of the example.
  • Table 26 shows the operating conditions of Model 032 electrostatic spray dryer used in the example.
  • Table 27 shows the water activity of the dried bacteria powders, determined using Rotronic equipment.
  • Table 28 shows the oil encapsulation efficiency of volatile oil powders produced with the ESD spray dryer system having either internal or external charge nozzles, and at relatively higher (140 °C) and lower (90 °C) inlet temperatures.
  • 1 g of powder was added to 9 g of water, and the solution was allowed to evaporate in a 130 °C oven for 60 hrs.

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Abstract

L'invention concerne un procédé de fourniture d'une poudre de composé actif consistant à sécher par pulvérisation électrostatique une formulation contenant au moins un composé actif, un agent d'encapsulation, et éventuellement un excipient à une température d'entrée de 150 °C ou moins et une température d'échappement de 100 °C ou moins, la charge électrique étant appliquée de manière externe à des gouttelettes de liquide de charge d'alimentation de formulation de composé actif.
PCT/US2023/017101 2022-03-31 2023-03-31 Poudres de composé actif séché par pulvérisation électrostatique et leur procédé de production WO2023192594A1 (fr)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2016123224A1 (fr) * 2015-01-28 2016-08-04 FONA Technologies, Inc. Encapsulation d'arôme faisant intervenir l'atomisation électrostatique
US10286411B2 (en) 2015-11-03 2019-05-14 Spraying Systems Co. Apparatus and method for spray drying
WO2020096908A1 (fr) * 2018-11-09 2020-05-14 FONA Technologies, Inc. Micro-encapsulation utilisant une atomisation par pulvérisation à courant alternatif haute fréquence, à faible courant et à haute tension
CN111387291A (zh) * 2019-02-13 2020-07-10 南昌大学 低温静电喷雾干燥生产油脂微胶囊的方法
WO2021102231A1 (fr) * 2019-11-21 2021-05-27 Spraying Systems Co. Produit laitier séché par pulvérisation électrostatique et son procédé de production

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2016123224A1 (fr) * 2015-01-28 2016-08-04 FONA Technologies, Inc. Encapsulation d'arôme faisant intervenir l'atomisation électrostatique
US10286411B2 (en) 2015-11-03 2019-05-14 Spraying Systems Co. Apparatus and method for spray drying
WO2020096908A1 (fr) * 2018-11-09 2020-05-14 FONA Technologies, Inc. Micro-encapsulation utilisant une atomisation par pulvérisation à courant alternatif haute fréquence, à faible courant et à haute tension
CN111387291A (zh) * 2019-02-13 2020-07-10 南昌大学 低温静电喷雾干燥生产油脂微胶囊的方法
WO2021102231A1 (fr) * 2019-11-21 2021-05-27 Spraying Systems Co. Produit laitier séché par pulvérisation électrostatique et son procédé de production

Non-Patent Citations (21)

* Cited by examiner, † Cited by third party
Title
"Determination of the Peroxide Value", IFRA ANALYTICAL METHOD
ALPIZAR-REYES ET AL., INTERNATIONAL JOURNAL OF BIOLOGICAL MACROMOLECULES, vol. 145, 2020, pages 207 - 215
ANWAR ET AL., JOURNAL OF FOOD ENGINEERING, vol. 105, 2011, pages 367 - 378
BAKRY ET AL., COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY, vol. 15, no. 1, 2008, pages 143 - 182
BENITO-ROMAN ET AL., HELIYON, vol. 6, no. 4, 2020, pages e03615 - e03615
DA SILVA JAMES ET AL., BRAZILIAN JOURNAL OF DEVELOPMENT, vol. 5, no. 7, 2019, pages 8082 - 95
DESAI ET AL., JOURNAL OF MICROENCAPSULATION,, vol. 22, no. 2, 2005, pages 179 - 192
DOMIAN ET AL., JOURNAL OF FOOD ENGINEERING, vol. 125, no. 1, 2014, pages 34 - 43
DUHAN ET AL., JOURNAL OF FOOD PROCESSING AND PRESERVATION, vol. 45, no. 6, 2021, pages e15537
ERATTE ET AL., JOURNAL OF FUNCTIONAL FOODS, vol. 19, 2015, pages 882 - 892
GUPTA ET AL., JOURNAL OF CHEMICAL AND PHARMACEUTICAL RESEARCH, vol. 7, no. 1, 2015, pages 568 - 572
HASHIM ET AL., MATERIALS TODAY: PROCEEDINGS, vol. 42, 2021, pages 222 - 228
HEE ET AL., THE JOURNAL OF SUPERCRITICAL FLUIDS, vol. 130, 2017, pages 118 - 124
JEYAKUMARI ET AL., JOURNAL OF FOOD SCIENCE AND TECHNOLOGY, vol. 53, no. 1, 2016, pages 856 - 863
JOHNSON R.K. ET AL: "Electrostatic-Enhanced Atomization for Spray Drying of Milk", LWT- FOOD SCIENCE AND TECHNOLOGY, vol. 29, no. 1-2, 1 January 1996 (1996-01-01), United Kingdom, pages 71 - 81, XP055779142, ISSN: 0023-6438, DOI: 10.1006/fstl.1996.0010 *
KAYA ET AL., FOOD SCIENCE AND TECHNOLOGY, vol. 141, 2021, pages 110872
KOUTSOPOULOS ET AL., MEAT SCIENCE, vol. 79, no. 1, 2008, pages 188 - 197
RAHMANI-MANGLANO ET AL., FOODS, vol. 9, no. 545, 2020, pages 21
SADEK ET AL., FOOD HYDROCOLLOIDS, vol. 48, 2015, pages 8 - 16
SELIM ET AL., MOLECULES, vol. 26, no. 6109, 2021, pages 17
SHANTHA ET AL., JOURNAL OF AOAC INTERNATIONAL, vol. 77, no. 2, 1994, pages 421 - 424

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