Popping crystal composition

Abstract

A composition comprising gas-filled crystals having a particle size of 0.2 mm to 0.85 mm, wherein a 250 mg sample of the gas-filled crystals exhibits a maximum dissolution rate of 0.6 Pa over 10 minutes of dissolution in water. rms * A composition that generates a cumulative burst signal over seconds.

Description

Technical Field

[0001] The present invention generally relates to nutritional supplement compositions, and more specifically, to nutritional supplement compositions having gas-filled popping crystals.

Background Art

[0002] Popping crystals are known in the confectionery industry and are often sold in various flavors as novelty candies. Popping crystals are typically made from sugar crystals having pressurized gas contained within cavities in the sugar crystals. When the sugar crystals are dissolved or crushed in a user's mouth, the pressurized gas is released, creating a fun "popping" sensation and sound in the user's mouth. While the popping sensation and sound are interesting and enjoyable, this confectionery form is used almost exclusively as a candy and not as a nutritional, health, or pharmaceutical dosage form. There are a number of reasons for this. For example, the average particle size of popping crystals is very large, greater than 1 mm in diameter and often as large as 4 mm in diameter. Additionally, the cavities in these sugar crystals hold a relatively large amount of pressurized gas, which creates a very pronounced popping sensation and sound over a long period of time, often lasting for more than a minute. Such intense properties are enjoyable as a novelty candy but are not suitable as a dosage form for frequently ingested nutritional, health, or pharmaceutical products. Further, the large particle size results in poor compositional uniformity when mixed with vitamins, minerals, active pharmaceutical ingredients ("APIs"), sweeteners, and other excipients.

[0003] Therefore, there is a need for a popping crystal-containing dosage form having improved physical properties that is suitable for frequently ingested nutritional, health, or pharmaceutical products.

Summary of the Invention

[0004] In one aspect, the composition includes gas - encapsulated crystals having a particle size of 0.2 mm to 0.85 mm, and a 250 - mg sample of the gas - encapsulated crystals produces a cumulative popping signal of up to 0.6 Pa over 10 minutes of dissolution in water. rms * seconds. In some embodiments, the cumulative popping signal is 0.2 to 0.6 Pa rms * seconds.

[0005] In some cases, the gas - encapsulated crystals include sugar; and a pressurized gas encapsulated within cavities in the gas - encapsulated crystals. The sugar includes glucose, fructose, sucrose, lactose, maltose, corn syrup, glucose syrup, or any combination thereof. In some examples, the sugar includes sucrose and glucose syrup. The gas - encapsulated crystals can further include an acidulant. In some cases, the acidulant is malic acid.

[0006] In some embodiments, the gas includes carbon dioxide, nitrogen, air, noble gas, or any combination thereof. The pressurized gas can have a pressure greater than 1 atmosphere in some examples.

[0007] In some cases, the gas - encapsulated crystals have a particle size of 0.5 to 0.7 mm.

[0008] In some embodiments, the composition further comprises one or more vitamins, minerals, biological activators, active pharmaceutical ingredients, or any combination thereof. Exemplary vitamins may include vitamin A, vitamin B (including B3, B6, B9, B12, and biotin), vitamin C, vitamin D, vitamin E, vitamin K, thiamine, riboflavin, niacin, folic acid, pantothenic acid, pharmaceutically acceptable salts thereof, or combinations thereof. Exemplary minerals may include iron, phosphorus, iodine, copper, chromium, molybdenum, chloride, sodium, magnesium, calcium, zinc, selenium, manganese, potassium, choline, silicon, pharmaceutically acceptable salts thereof, or any combination thereof. Exemplary biological activators may include lycopene, lutein, L-threonine, coenzyme Q-10, plant sterols, hyaluronic acid, cognitive citicoline, nicotinamide, andrography, or any combination thereof. Exemplary active pharmaceutical ingredients may include pain or inflammation reducers, antihistamines, decongestants, cough suppressants, biological activators, sleep aids, stress reducers, energy and cognitive aids, Ayurvedic supplements, immune supplements, digestive aids, joint supplements, cannabinoids, systemic natural substances, nutritional supplements, pharmaceutically acceptable salts thereof, or combinations thereof.

[0009] In some embodiments, the composition further comprises a sweetener. In some cases, the sweetener comprises glucose, fructose, sucrose, lactose, maltose, corn syrup, or any combination thereof.

[0010] The composition may further contain diluents, flavorings, colorings, preservatives, or any combination thereof.

[0011] In another embodiment, the composition comprises gas-filled crystals having a particle size of 0.25 to 0.85 mm, the gas-filled crystals comprising sucrose, glucose syrup, and pressurized gas sealed in cavities within the gas-filled crystals, and a 250 mg sample of the gas-filled crystals dissolves in water for 10 minutes at a pressure of 0.2 to 0.6 Pa. rms * A burst signal is produced in seconds. The gas is carbon dioxide pressurized to over 1 atmosphere in some cases. The composition may further include, in some examples, one or more vitamins, minerals, biological activators, active pharmaceutical ingredients, or any combination thereof. In some embodiments, the composition further includes an acidulant. An exemplary acidulant is malic acid. [Brief explanation of the drawing]

[0012] [Figure 1] This is a block diagram of the method for preparing gas-filled crystals. [Figure 2] This is a perspective view of the sound system. [Figure 3] Figure 2 is a cross-sectional view of the acoustic device. [Figure 4] This is a perspective view of the sample wetting cup. [Figure 5] Figure 4 is a side view of the sample wetting cup. [Figure 6] Figure 4 is a top view of the sample wetting cup. [Figure 7] Figure 4 is a bottom view of the sample wetting cup. [Figure 8] Figure 5 is a vertical cross-sectional view of the sample wetting cup. [Figure 9] This is a vertical cross-sectional view of the sample wetting cup shown in Figure 5, connected to the fluid injection nozzle. [Figure 10] Figure 4 is a photograph of the sample wetting cup containing the sample before the addition of the wetting fluid. [Figure 11] Figure 10 is a photograph of the sample wetting cup after the sample has been dissolved in water. [Figure 12] Figure 10 is a photograph of a sample wetting cup with drainage holes. [Figure 13]This graph shows the mixing uniformity of a composition containing relatively large gas-filled crystals. [Figure 14] This graph shows the mixing uniformity of a composition containing relatively small gas-filled crystals. [Figure 15] This plot shows the cumulative rupture signal of gas-filled crystals with various particle size ranges. [Figure 16] This plot shows comparative data of cumulative burst signals for gas-filled crystals with various particle sizes and for novel commercially available candies. [Modes for carrying out the invention]

[0013] The embodiments described herein can be more readily understood by referring to the following detailed description, examples, and drawings. However, the elements, apparatus, and methods described herein are not limited to the specific embodiments presented in the detailed description, examples, and drawings. It should be understood that the exemplary embodiments herein are merely illustrative of the principles of the invention. Numerous modifications and adaptations will be readily apparent to those skilled in the art without departing from the spirit and scope of the invention.

[0014] In addition, all scopes disclosed herein are understood to encompass any and all subscopes contained therein. For example, the scope “1.0–10.0” described herein is considered to include any and all subscopes beginning with a minimum value of 1.0 or greater and ending with a maximum value of 10.0 or less, such as 1.0–5.3, or 4.7–10.0, or 3.6–7.9.

[0015] All scopes disclosed herein are also to be considered to include the endpoints of the scope unless it is clearly stated otherwise. For example, the scopes “between 5 and 10,” or “5 to 10,” or “5-10” are generally considered to include the endpoints 5 and 10.

[0016] The units for "percentages based on weight" are interchangeable as "weight%" or "wt.%" unless otherwise clearly stated.

[0017] It will be further understood that one or more features of one embodiment may be broadly applied to other embodiments, even if not specifically described or illustrated in such other embodiments, unless explicitly prohibited by the nature of the disclosure or the related embodiments. Similarly, compositions and methods described herein may include any combination of features and / or steps described herein that are not inconsistent with the purpose of the disclosure. Numerous modifications and / or adaptations of compositions and methods described herein will be readily apparent to those skilled in the art without departing from the subject matter of the invention.

[0018] Compositions suitable as nutritional, health, or pharmaceutical supplements are described herein. In one embodiment, the composition is an edible composition comprising gas-filled crystals. As described in more detail in Example 1, consumer preference studies found that consumers enjoyed the popping sensation and sound produced by gas-filled crystals found in novel candies, but the intensity and duration of the popping sensation were too strong and long, making it difficult to regularly consume such products as part of a nutritional, health, or pharmaceutical regimen. However, additional studies found that consumers preferred reduced popping intensity and duration. Specifically, the most preferred composition was found to contain gas-filled crystals having a specific particle size distribution of 0.2 to 0.85 mm. In particular, as described in more detail herein, gas-filled crystals having a particle size of 0.2 to 0.85 mm, wherein a 250 mg sample of the gas-filled crystals exhibited a maximum of 0.6 Pa over 10 minutes of dissolution in water. rms * It was found that the gas-filled crystal that produced a cumulative burst signal over seconds was the most preferable.

[0019] Furthermore, in addition to having the desired cumulative burst signal, the gas-filled crystal particle size range of 0.2 to 0.85 mm was found to have excellent mixing uniformity characteristics. As described in more detail in Example 2, when the composition has larger gas-filled crystals (e.g., greater than 0.85 mm, e.g., 0.85 mm to 4 mm), other components in the composition easily separate from the gas-filled crystals, resulting in insufficient mixing uniformity.

[0020] These gas-filled crystals may further contain one or more vitamins, minerals, biological activators, APIs, or any combination thereof; and additional excipients such as acidulants, acidifying agents, flavorings, diluents, colorants, preservatives, or any combination thereof.

[0021] Compositions, methods for producing the compositions, and devices and analytical methods for determining the intensity and duration of the bursting sensation of gas-filled crystals are described herein. I. Composition

[0022] In one embodiment, the composition described herein is an edible composition containing gas-filled crystals. In some embodiments, the gas-filled crystals in the composition have a particle size of 0.25 to 0.85 mm. In some cases, the gas-filled crystals have particle sizes of 0.25 to 0.8 mm, 0.25 to 0.75 mm, 0.25 to 0.7 mm, 0.25 to 0.65 mm, 0.25 to 0.6 mm, 0.25 to 0.55 mm, 0.25 to 0.5 mm, 0.25 to 0.45 mm, 0.25 to 0.4 mm, 0.25 to 0.35 mm, 0.25 to 0.3 mm, 0.3 to 0.85 mm, 0.35 to 0.85 mm, 0.4 to 0.85 mm, 0.45 to 0.85 mm, 0.5 to 0.85 mm, The particles have a particle size of 0.55-0.85 mm, 0.6-0.85 mm, 0.65-0.85 mm, 0.7-0.85 mm, 0.8-0.85 mm, 0.3-0.8 mm, 0.35-0.75 mm, 0.4-0.7 mm, 0.45-0.65 mm, 0.5-0.65 mm, 0.5-0.6 mm, 0.55-0.65 mm, 0.5-0.66 mm, 0.5-0.7 mm, 0.45-0.75 mm, 0.45-0.7 mm, or 0.45-0.65 mm.

[0023] In some embodiments, the gas-filled crystals are present in amounts of 5%~60%, 5%~55%, 5%~50%, 5%~45%, 5%~40%, 5%~35%, 5%~30%, 5%~25%, 5%~20%, 5%~15%, 5%~10%, 10%~60%, 15%~60%, 20%~60%, 25%~60%, and 30%~60% by weight of the composition. It is present in the composition in amounts of %, 35%~60%, 40%~60%, 45%~60%, 50%~60%, 55%~60%, 10%~55%, 15%~50%, 20%~45%, 25%~40%, 30%~35%, 5%, 10%, 15%, 20%, 25%, 30%, 35%, 40%, 45%, 50%, 55%, or 60%.

[0024] In some examples, gas-filled crystals contain sugar and pressurized gas sealed within the cavities of the gas-filled crystal. The term “sugar” includes monosaccharides, disaccharides, polysaccharides, sugar alcohols, or any combination thereof. Monosaccharides as described herein may include fructose, glucose, or any combination thereof. Disaccharides as described herein may include sucrose, lactose, maltose, or any combination thereof. Polysaccharides as described herein may include syrups, such as glucose syrup, corn syrup, high-fructose corn syrup, agave syrup, high-maltose syrup, rice syrup (such as brown rice syrup), or any combination thereof. Sugar alcohols as described herein may include erythritol, sorbitol, xylitol, mannitol, or any combination thereof.

[0025] In some cases, sugars include glucose, fructose, sucrose, lactose, maltose, glucose syrup, corn syrup, or any combination thereof. In some examples, sugars include sucrose and glucose syrup.

[0026] The amount of sugar present in the gas-filled crystal may be any amount not inconsistent with the purposes of this disclosure. For example, in some cases, the gas-filled crystal may contain 90–99.9% sugar. In some examples, the gas-filled crystal may contain, by weight, 91–99.9%, 92–99.9%, 93–99.9%, 94–99.9%, 95–99.9%, 96–99.9%, 97–99.9%, 98–99.9%, 99–99.9%, 91%, 92%, 93%, 94%, 95%, 96%, 97%, 98%, 99%, or more than 99% but less than 100% sugar.

[0027] The pressurized gas sealed within the cavities of the gas-filled crystal includes an inert gas. The term "inert" means a gas that does not chemically react with any vitamin, mineral, or API present in the material forming the gas-filled crystal (such as sugar) or in the composition, whether the vitamin, mineral, or API is present in the gas-filled crystal material on its own or as a mixture with the gas-filled crystal. Examples of gases include carbon dioxide, nitrogen, air, noble gases, or any combination thereof.

[0028] In some embodiments, the term "pressurization" refers to a pressure exceeding 1 atmosphere. In some cases, the term "pressurization" refers to a pressure greater than the ambient pressure outside the cavity within the gas-filled crystal.

[0029] The pressurized gas can be released from the cavities in the gas-filled crystal, creating a bursting sensation and sound that the user experiences when the gas-filled crystal dissolves in water, comes into contact with saliva in the consumer's mouth, and / or when the gas-filled crystal is crushed during chewing. As described in more detail in Sections III and IV herein, the cumulative bursting signal can be measured against the gas-filled crystal during dissolution of the gas-filled crystal by water. Specifically, the cumulative bursting signal can be determined with respect to the intensity of the desired bursting sensation, such as for gas-filled crystals having a predetermined particle size range identified as preferred by consumers in the consumer study discussed in Example 1. In some embodiments, a 250 mg sample of the gas-filled crystals described herein produces a cumulative bursting signal of up to 0.6 Pa rms * seconds over a 10-minute dissolution by water. In some cases, a 250 mg sample of the gas-filled crystals produces a cumulative bursting signal of up to 0.55 Pa rms * seconds, up to 0.5 Pa rms * seconds, up to 0.45 Pa rms * seconds, up to 0.4 Pa rms * seconds, up to 0.35 Pa rms * seconds, up to 0.3 Pa rms * seconds, up to 0.25 Pa rms * seconds, up to 0.2 Pa rms * seconds, 0.2 - 0.6 Pa rms * seconds, 0.25 - 0.6 Pa rms * seconds, 0.3 - 0.6 Pa<0**********> * seconds, 0.35 - 0.6 Pa rms * [[ID=********]]seconds, 0.4 - 0.6 Pa rms * seconds, or 0.5 - 0.6 Pa rms * seconds.

[0030] In some embodiments, the composition may further contain a sweetener. In some cases, the sweetener is a natural sugar, including glucose, fructose, sucrose, lactose, maltose, corn syrup, yacon syrup, monk fruit, honey, agave, coconut sugar, date sugar, fruit puree, fruit juice, maple syrup, molasses, or any combination thereof. In some examples, the sweetener may also be an artificial sweetener, such as stevia, erythritol, xylitol, allulose, acesulfame K, aspartame, neotame, saccharin, sucralose, or any combination thereof. Additionally, in some embodiments, it is also considered that a combination of natural sugars and artificial sweeteners may be used. The amount of sweetener present in the composition may be any amount not inconsistent with the purposes of this disclosure. In some cases, sweeteners make up 10%-80%, 10%-75%, 10%-70%, 10%-65%, 10%-60%, 10%-55%, 10%-50%, 10%-45%, 10%-40%, 10%-45%, 10%-40%, 10%-35%, 10%-30%, 10%-25%, 10%-20%, 10%-15%, 15%-80%, 20%-80%, 25%-80%, and 30% by weight of the composition. It is present in the composition in amounts of %~80%, 35%~80%, 40%~80%, 45%~80%, 50%~80%, 55%~80%, 60%~80%, 65%~80%, 70%~80%, 15%~60%, 20%~55%, 25%~50%, 30%~45%, 10%, 15%, 20%, 25%, 30%, 35%, 40%, 45%, 50%, 55%, 60%, 65%, 70%, 75%, or 80%.

[0031] The composition may further contain one or more vitamins, minerals, biological activators, APIs, or any combination thereof. In some cases, the composition contains one or more vitamins, minerals, biological activators, APIs, or any combination thereof mixed with a gas-filled crystal. In some examples, the composition contains a gas-filled crystal containing one or more vitamins, minerals, APIs, or any combination thereof. In some embodiments, each of the one or more vitamins, minerals, biological activators, and APIs may be present in the composition both mixed with the gas-filled crystal and incorporated within the gas-filled crystal.

[0032] Vitamins, minerals, or biological activators include vitamin A, vitamin B (including B3, B6, B9, B12, and biotin), vitamin C, vitamin D, vitamin E, vitamin K, thiamine, riboflavin, niacin, folic acid, pantothenic acid, iron, phosphorus, iodine, copper, chromium, molybdenum, chloride, sodium, magnesium, calcium, zinc, selenium, manganese, potassium, choline, lycopene, lutein, L-threonine, coenzyme Q-10, plant sterols, hyaluronic acid, cognitive citicoline, nicotinamide, andrographica, pharmaceutically acceptable salts thereof, or combinations thereof.

[0033] In some embodiments, the API includes pain or inflammation reducers, antihistamines, decongestants, cough suppressants, bioactive agents, sleep aids, stress reducers, energy and cognitive aids, Ayurvedic supplements, immune supplements, digestive aids, joint supplements, cannabinoids, systemic natural substances, nutritional supplements, pharmaceutically acceptable salts thereof, or combinations thereof.

[0034] Exemplary pain- or inflammation-reducing agents include ibuprofen, naproxen, acetaminophen, salicylic acid, acetylsalicylic acid, ketoprofen, dexibuprofen, fenoprofen, dexketoprofen, flurbiprofen, oxaprozin, loxoprofen, diflunisal, etodolac, indomethacin, ketorolac, piroxicam, salsalate, salicylic acid, indomethacin, tolmetin, sulindac, etodolac, ketorolac, diclofenac, aceclofenac, bromfenac, pharmaceutically acceptable salts thereof, or combinations thereof.

[0035] Antihistamines include cetirizine hydrochloride, levocetirizine hydrochloride, loratadine, desloratadine, fexofenadine hydrochloride, azelastine hydrochloride, olopatadine hydrochloride, brompheniramine maleate, chlorcyclizine hydrochloride, chlorpheniramine maleate, dexbrompheniramine maleate, dexchlorpheniramine maleate, diphenhydramine citrate, diphenhydramine hydrochloride, doxylamine succinate, phenindamine tartrate, pheniramine maleate, pyriramine maleate, tondylamine hydrochloride, triprolidine hydrochloride, pharmaceutically acceptable salts thereof, or combinations thereof.

[0036] Decongestive or cough suppressants include phenylephrine hydrochloride, pseudoephedrine hydrochloride, pseudoephedrine sulfate, phenylephrine ditartrate, dextromethorphan, holcodin, codeine, benzonate, pharmaceutically acceptable salts thereof, or combinations thereof.

[0037] Sleep aids may contain melatonin, lemon balm, lavender, chamomile, sage, valerian root extract, hops, passionflower extract, or a combination thereof.

[0038] Stress-reducing aids containing sage, ashwagandha (Withania somnifera), St. John's wort, GABA (gamma-aminobutyric acid), or a combination thereof.

[0039] An energy and cognitive aid containing green tea, Korean ginseng, caffeine, Rhodiola rosea extract, B vitamin, L-theanine, taurine, pharmaceutically acceptable salts thereof, or combinations thereof.

[0040] Ayurvedic supplements include amla (Emblica officinalis), bibhitaki (Terminalia bellirica), haritaki (Terminalia chebula), brahmi, cumin, licorice, gotu kola, cardamom, or a combination thereof.

[0041] The immune supplement contains copper, silver, spirulina, astragalus, beta-glucan, acerola fruit extract, blood orange extract, elderberry, mushrooms (Lion's Mane, Lychee, Shiitake, Cordyceps), pharmaceutically acceptable salts thereof, or any combination thereof.

[0042] Digestive aids include probiotics and combinations thereof; digestive enzymes; soluble fibers including psyllium husk, inulin, fenugreek fiber, and wheat dextrin; cascara sagrada; aloe ferox leaf extract, slippery elm bark extract, or combinations thereof.

[0043] Joint supplements may contain collagen, glucosamine, turmeric, methylsulfonylmethane (MSM), their pharmaceutically acceptable salts, or combinations thereof.

[0044] Cannabinoids include cannabidiol, cannabigerol, their pharmaceutically acceptable salts, and combinations thereof.

[0045] The systemic natural substances include one or more of the following: Boswellia, curcumin, devil's claw, ginger, feverfew, bromelain, turmeric, and butterbur.

[0046] The nutritional supplement contains black pepper, glycine, valerian root, eucalyptus, menthol, astragalus, bromelain, echinacea, white willow, ivy leaves (Hedera helix), ginger (Zingiber officinale), pharmaceutically acceptable salts thereof, or combinations thereof.

[0047] The compositions described herein may further include additional excipients such as acidulants, diluents, flavorings, colorants, preservatives, or any combination thereof.

[0048] Examples of acidulants include malic acid, citric acid, turmeric acid, lactic acid, tartaric acid, acetic acid, sodium ascorbate, ascorbic acid, succinic acid, or combinations thereof. In some embodiments, the acidulant is malic acid. In some cases, the composition comprises one or more acidulants mixed with gas-filled crystals. In some examples, the composition comprises gas-filled crystals containing one or more acidulants. In some embodiments, one or more acidulants are present in the composition both mixed with the gas-filled crystals and incorporated within the gas-filled crystals.

[0049] Examples of diluents include maltodextrin, starch, cellulose, sugar, fiber, or any combination thereof. If present, the amount of diluent may be any amount not inconsistent with the purposes of this disclosure.

[0050] Flavorings may be used in the composition as an option. If present, the flavorings may be any flavorings known in the art that are not inconsistent with the purposes of this disclosure. As is known to those skilled in the art, the amount of flavoring present will depend on the desired flavor, the specific flavoring used, and whether the flavoring is a component of the gas-filled crystal material or present separately as a mixture in the composition. In some cases, the composition includes flavorings mixed with the gas-filled crystal. In some embodiments, the composition includes gas-filled crystals containing flavorings. In some embodiments, the flavorings are present in the composition both mixed with the gas-filled crystal and incorporated into the gas-filled crystal.

[0051] Optionally, colorants may be used in the composition. If present, the colorant may be any colorant known in the art that is not inconsistent with the purposes of this disclosure. As is known to those skilled in the art, the amount of colorant present will depend on the desired color, the specific colorant used, and whether the colorant is a component of the gas-filled crystal material or present separately as a mixture in the composition. In some cases, the composition includes a colorant mixed with the gas-filled crystal. In some embodiments, the composition includes a gas-filled crystal containing a colorant. In some embodiments, the colorant is present in the composition both mixed with the gas-filled crystal and incorporated into the gas-filled crystal.

[0052] In some examples, preservatives are present in the composition. The preservatives may be any preservative that is not inconsistent with the purposes of this disclosure. Exemplary preservatives include sodium benzoate, benzyl alcohol, methylparaben, propylparaben, or any combination thereof. The preservatives may be present in the composition in any amount that is not inconsistent with the purposes of this disclosure. In some cases, the composition comprises a preservative mixed with gas-filled crystals, and in other cases, the composition comprises gas-filled crystals containing a preservative. In some embodiments, the preservative is present in the composition both mixed with the gas-filled crystals and incorporated into the gas-filled crystals. II. Method for Manufacturing Compositions

[0053] In another embodiment, a method for preparing the compositions disclosed in Section I of this specification is described. In some embodiments, gas-filled crystals can be prepared using methods known in the art. For example, U.S. Patents 3,985,909, 3,985,910, 4,001,457, and 4,289,794 describe methods for producing gas-filled crystals. As shown in Figure 1, a method for preparing gas-filled crystals includes the steps of: generating a sugar melt at an elevated temperature 200; introducing the heated sugar melt into a pressure vessel 201; introducing an inert gas into the pressure vessel at above atmospheric pressure 202; dispersing the gas into the heated sugar melt through stirring 203; cooling the gas-filled sugar melt to form a gas-filled solid sugar matrix 204; crushing the gas-filled solid sugar matrix into gas-filled crystals by impact treatment 205; and passing the gas-filled crystals through one or more sieves 206 to obtain a desired particle size range and / or distribution.

[0054] The compositions described in Section I can be prepared by mixing gas-filled crystals with a sweetener, additional excipients, and one or more vitamins, minerals, and / or APIs. III. Analyzer

[0055] In the embodiments shown in Figures 2 and 3, the acoustic device 100 includes a soundproof container 110 having a closable door 111, a sample receiving platform 112, and sound-reducing sound-insulating material 120 lining the inward-facing surfaces of the walls including the soundproof container 110 and the door 111. The exemplary sound-reducing sound-insulating material may include an acoustic foam having or not having a sound-reducing surface pattern such as an "eggshell" pattern, or any other sound-reducing sound-insulating material that is not inconsistent with the purposes of this disclosure. In the embodiment of Figure 2, the closable door 111 is located on one of the vertical sides of the container 110. However, in other cases, the door 111 may be located as a lid on the upper horizontal wall 110a of the container 110. The container 110 may be cubic or rectangular in shape with a centrally located internal receiving space 130. A removable wetting cup 1 is located on the sample receiving platform 112 in the internal receiving space 130. The sample receiving platform 112 has a first receiving hole through which the wetting cup 1 is placed. As will be discussed in more detail below, the wetting cup 1 is positioned such that the fluid receiving hole 40 in the wetting cup 1 is aligned with the first receiving hole.

[0056] The vibration-damping foot 113 can be optionally placed on the outer surface of the bottom horizontal wall 110b of the container 110. The foot 113 can be made from any vibration-absorbing or damping material that is not inconsistent with the purposes of this disclosure, such as natural or synthetic rubber. Generally, the purpose of the vibration-damping foot 113 is to reduce external vibrations sensed by the acoustic device 100. In addition to or in the absence of the vibration-damping foot 113, the acoustic device 100 can be placed on a vibration-resistant surface, which can be used together with or in place of the vibration-damping foot 113.

[0057] The second receiving hole passes through the upper horizontal wall 110a and the sound-insulating section 120 located thereon. A microphone 140 or other measuring device can be placed in the second receiving hole. In the embodiments shown in Figures 2 and 3, the microphone 140 passes through the second receiving hole and extends into the internal receiving space 130. In some examples, the first receiving hole, the second receiving hole, and the fluid receiving hole 40 are roughly aligned along a common axis A, while in other embodiments, the holes are arranged in a configuration other than along axis A. In some embodiments, the microphone 140 is positioned roughly above the center of the wetting cup 1. In other cases, the second receiving hole may pass through one of the vertical side walls of the container 110, and the microphone 140 extends horizontally into the internal receiving space 130.

[0058] In the embodiments shown in Figures 4 to 11, the wetting cup 1 comprises a fluid receiving bowl 10; a fluid overflow base 20; a fluid receiving space 30 located within the fluid receiving bowl 10; and a fluid receiving hole 40. The fluid receiving bowl 10 has a circumferentially extending shelf portion 11 located on an inward-facing surface adjacent to the edge of the fluid receiving bowl 10. A frit-like disc 60 can be placed on the shelf portion 11, covering the fluid receiving space 30. The frit-like disc 60 can be made from glass, a polymer, or any other material not inconsistent with the purposes of this disclosure. In the embodiment shown in Figure 8, the outer surface of the frit-like disc 60 may be at the same height as the edge of the fluid receiving bowl 10. In another embodiment shown in Figure 9, the outer surface of the frit-like disc 60 may extend further outward from the edge of the fluid receiving bowl 10. In examples where capillary action is used to transport the fluid from the fluid receiving bowl 10 to the outer surface of the frit-like disc 60 and bring it into contact with the sample 70, the embodiment shown in Figure 9 is commonly used.

[0059] In some embodiments, the fluid overflow base 20 has a bottom surface 50 that can be placed on a sample receiving platform 112 in the internal receiving space 130 of the acoustic device 100. In some examples, the bottom surface 50 is flat. The nozzle 41 can be detachably connected to the fluid receiving hole 40, for example, via a friction fitting or screw fastening mechanism. In other cases, the nozzle 41 is integrally formed as part of the fluid overflow base 20 and extends outward from the bottom surface 50. For example, as shown in Figure 9, the nozzle 41 can be connected to the fluid receiving hole 40, and a fluid conduit 42, such as a tube, can be connected to the end of the nozzle 41. The fluid conduit 42 can connect the nozzle 41 to a fluid distribution device, such as a syringe or other known fluid distribution device (not shown).

[0060] As shown in Figure 3, the wetting cup 1 can be positioned on the sample receiving platform 112 such that the fluid receiving hole 40 and the first receiving hole are aligned along axis A. The fluid conduit 42 can be connected to a fluid distribution device (such as a syringe) via a nozzle 41, allowing a known volume of fluid to pass through the fluid conduit 42 and nozzle 41 to fill the fluid receiving space 30 of the fluid receiving bowl 10. As the fluid rises in the fluid receiving bowl 10, it can come into contact with the frit-like disc 60. As long as the wetting cup 1 is horizontal, the fluid will come into uniform contact with the bottom surface of the frit-like disc 60, be drawn up through the frit-like disc 60, and wet the outer surface of the frit-like disc 60 in a uniform manner. Subsequently, by capillary action, the fluid will be pumped out through the frit-like disc 60, uniformly wetting the surface of the frit-like disc 60. As shown in Figures 10 and 11, the sample 70 can be placed on the outer surface of the frit-like disc 60. A fluid (such as water or a solvent) can be injected into the fluid receiving space 30 of the bowl 10, and when the fluid comes into contact with the bottom of the frit-like disc 60, the fluid is drawn into the frit-like disc 60 via capillary action and comes into contact with the sample 70.

[0061] As shown in Figure 11, the volume of fluid injected into the fluid receiving space 30 can be greater than the volume of the fluid receiving space 30 to ensure that the frit-like disc 60 is completely saturated and wetted by the fluid. Any excess fluid can overflow the edge of the fluid receiving bowl 10 and be captured by the fluid overflow base 20. In some cases, a fixed volume of fluid can be injected into the fluid receiving space 30. In other cases, a continuous flow of fluid can be injected into the fluid receiving space 30. When a continuous flow of fluid is used, a drain hole 43 can be formed in the fluid overflow base 20 to discharge excess fluid. Similar to the fluid receiving hole 40, the drain hole 43 can be connected to a second nozzle 41 and a second fluid conduit 42 to discharge the fluid away from the wetting cup 1. IV. Analysis methodology

[0062] In another embodiment, the acoustic device 100 can be used to measure the intensity and / or duration of the bursting sensation of a gas-filled crystal when it dissolves in water. Specifically, the acoustic device 100 measures Pascals RMS seconds (Pa rms * It can be used to determine the cumulative burst signal over time, expressed in units of seconds (RMS means root mean square). In some embodiments, the RMS time is defined as 250 RMS data points per second (or RMS over 0.004 s). Those skilled in the art will understand that the RMS time may be any RMS time that is not inconsistent with the purposes of this disclosure, and that the RMS time will depend on the physical properties of the sample 70 under test, the type and sensitivity of the microphone 140, the software used to process the data, the objectives of the experiment, etc.

[0063] In the embodiment, the acoustic device 100 is set up using a microphone 140 as described in Section III. An exemplary method for determining the cumulative burst signal over time is as follows: placing a sample 70 of a known amount of gas-filled crystals on a frit-like disc 60; positioning the microphone 140 above the sample 70 at a known fixed distance; injecting fluid into a wetting cup 1 to wet the frit-like disc 60; recording the burst sound intensity from the gas-filled crystals dissolved in the fluid over time intervals and converting the recorded burst sounds from voltage response units to pressure (Pa) units; subtracting the background signal from the total signal; and calculating the area under the curve of the signal by multiplying the background-corrected signal by the RMS time step and summing each time step over the entire test. [Examples]

[0064] Example 1 Consumer preference research - intensity and duration of burst sensation

[0065] A first consumer preference study was conducted with 178 participants to measure the sensory desirability of gas-encapsulated crystal formulations. Each participant consumed one flavored formulation containing gas-encapsulated crystals with a particle size of 0.5 mm to 1.0 mm daily for three days. Participants ranged in age from 18 to 65 years and were 50% male / 50% female. Two of the physical properties evaluated were burst intensity and burst duration. It was found that 25% of participants felt the burst sensation was too strong for daily consumption, and 21% stated that the burst sensation lasted too long, with approximately 10 seconds being considered the most desirable duration.

[0066] A second consumer preference study was conducted with 372 participants using a modified formulation containing half the amount of gas-filled crystals (to reduce the duration of the popping sensation) and having a narrower particle size (0.5-0.6 mm) (to reduce the intensity of the popping sensation). The intensity of the popping sensation and the duration of the popping sensation were two of the properties evaluated. 77% of participants felt that the duration of the popping sensation was just right (less than 10 seconds), while only 8% felt that the duration was too long. Additionally, 81% preferred the intensity of the popping sensation.

[0067] A third consumer preference study was conducted with 58 participants using the same formulation as the second consumer preference study, except that the gas-filled crystals had a particle size of 0.55 mm to 0.66 mm. The intensity of the popping sensation and the duration of the popping sensation were two of the physical properties evaluated. In this study, participants consumed one flavored formulation containing gas-filled crystals with a particle size of 0.54 mm to 0.66 mm. Only 4% of participants felt the popping sensation was too strong for daily consumption, and no participants felt the duration of the popping sensation was too long.

[0068] As a result, by reducing the particle size of the gas-filled crystals to a narrower particle size window that does not contain crystals larger than 0.66 mm and / or 0.85 mm, the intensity and duration of the burst sensation were significantly improved beyond those found in the first consumer preference study using gas-filled crystals with particle sizes larger than 0.85 mm. Example 2 Consumer preference research - Particle size range and product uniformity

[0069] When gas-filled crystals are used in nutritional, health, or pharmaceutical products where they are mixed with additional ingredients such as vitamins, minerals, biological activators, APIs, or sweeteners, the uniformity of the mixture of these ingredients is important for achieving the appropriate dosage and for preventing the accumulation and separation of individual ingredients.

[0070] It has been found that gas-filled crystals with relatively large particle sizes present problems when mixed with other additional components. Specifically, it has been found that gas-filled crystals with particle sizes exceeding 0.85 mm cannot be properly mixed with other components to produce a uniform distribution of gas-filled crystals. However, it has been found that gas-filled crystals with particle sizes of 0.85 mm or less produce an improved uniform distribution of gas-filled crystals with other components.

[0071] For example, a first-scale study batch containing 700 mg of gas-filled crystals, ranging in size from 0.5 mm to 1.0 mm, was prepared, mixed with 5 mg of zinc, 500 mg of vitamin C, 0.5 mg of manganese, 2 mg of vitamin B6, 0.012 mg of vitamin B12, 0.015 mg of vitamin D3, 0.1 mg of folic acid, 100 mg of tapioca maltodextrin, 2500 mg of fructose, and 55 mg of orange flavoring. As shown in Figure 13, the relatively large gas-filled crystals resulted in insufficient product uniformity in the mixture.

[0072] A second study-scale batch was prepared, having the same serving size as the first study-scale batch, but differing in that the 700 mg gas-filled crystals had a particle size of 0.54 mm to 0.66 mm. As shown in Figure 14, the relatively smaller particle size resulted in a dramatic improvement in the mixing of gas-filled crystals with additional components compared to gas-filled crystals with relatively larger particle sizes. Example 3 Measurement of cumulative rupture signal

[0073] Time-dependent cumulative rupture signal (Pa rms *To determine the time domain (seconds), a response curve is created using the acoustic apparatus 100 described in Section III and the method described in Section IV of this specification. Specifically, a filling syringe is attached to the acoustic apparatus and filled with approximately 50 mL of water. The microphone is placed in the internal receiving space of the acoustic apparatus and adjusted to 51 mm from the top of the frit-like disc (145-174 μm) on the wetting cup. To ensure repeatability of wetting, a 1-inch dosing ring is placed on the frit-like disc and a sample of gas-filled crystals (0.250 g ± 0.002 g) is uniformly placed in the dosing ring. Subsequently, water is injected into the wetting cup and audio recording is started at a known sampling rate (e.g., 192 ks / s) for a predetermined duration (e.g., 10 minutes). The amount of water injected into the wetting cup will depend on the volume of the fluid receiving space in the fluid receiving bowl of the wetting cup. As previously discussed herein, typically the volume of water injected will slightly exceed the volume of the fluid receiving space, such that some water overflows from the fluid receiving bowl into the fluid overflow base.

[0074] After recording is complete, each .wav file (raw data from each experiment) is exported from the microphone input path to the file input path to provide the voltage RMS response ("Vrms", 250 times per second) from the file over time. To do this, a high-pass filter (elliptic 800Hz) and a low-pass filter (Butterworth 20kHz) are applied, the RMS interval is set to 250 / s, and all units are set to Vrms. Subsequently, the data is exported and each Vrms is converted to pressure (Pa) units by applying the microphone sensitivity from the calibration sheet provided by the manufacturer. For the microphone used in this experiment, this is 50.79mV / Pa (e.g., 0.05079V / (50.79mV / Pa / 1000) = 1Pa). rms )

[0075] Next, we calculate the average background noise. This is done by averaging the first 5 seconds of the recording (Pa rms (Units). Next, background Pa rmsAverage, background Pa rms Standard deviation, and background Pa rms average +3 * Calculate the standard deviation.

[0076] Next, the background correction signal is determined by subtracting the background signal from the total signal. First, each Pa rms Regarding this, the signal is background average +3 * Determine whether it is greater than the standard deviation. If so, the signal can be distinguished from the background. rms If the signal can be distinguished from the background noise, the background is subtracted to determine the background correction signal. However, it should be noted that if the background and signal are not in phase or have the same frequency, simple subtraction of the signal is not possible. Calculation of background correction signal = (Sqrt(Total signal) 2 - background 2 ).

[0077] To calculate the area under the curve, the background correction signal is multiplied by the RMS time step (0.004 s). Then, each time step is summed up over the entire test to obtain the total area under the curve (Pa). rms * Get seconds. Example 4 Cumulative rupture signal - particle size range

[0078] The cumulative rupture signals for gas-filled crystals with various particle size ranges were determined using the method described in Example 3. In this experiment, the microphone used was a GRAS146AE from GRAS Sound & Vibration, and the audio analyzer was an Apx517B from Audio Precision.

[0079] Three samples of gas-filled crystals with different particle size ranges were prepared: Sample 1 was 0.546 mm to 0.66 mm, Sample 2 was 0.6 mm to 0.85 mm, and Sample 3 was 0.85 mm to 1.00 mm. Nine replicates were prepared and tested for Samples 1 and 2, and eight replicates for Sample 3. Each sample was approximately 250 mg, and audio recordings for each replicate were made for 10 minutes. To account for some variation caused by ambient conditions, testing was performed by testing batches of two or three replicates daily over three days.

[0080] Figure 15 shows the signal area (Pa) for each of samples 1-3. rms * The graph shows the results over 10 minutes. As shown, for both Sample 1, which has gas-filled crystals with a particle size of 0.546 mm to 0.66 mm, and Sample 2, which has gas-filled crystals with a particle size of 0.6 mm to 0.85 mm, both were subjected to 0.6 Pa over 10 minutes. rms * It showed a cumulative rupture signal of less than 10 seconds. In contrast, sample 3, which had gas-filled crystals with a particle size of 0.85 mm to 1.00 mm, showed 0.6 Pa over 10 minutes. rms * It showed a cumulative rupture signal exceeding a few seconds.

[0081] I don't intend to get bogged down in theory, but 0.6 Pa over 10 minutes rms * Based on the cumulative signal area of ​​less than 1 second (as shown in Figure 15), gas-filled crystals with a particle size of 0.2 mm to 0.85 mm are considered to produce a more consumer-preferred burst intensity upon dissolution with water. In contrast, gas-filled crystals with a particle size of 0.85 mm to 1 mm (or larger) over 10 minutes at 0.6 Pa rms * The change in cumulative signal area over several seconds may result in consumers disliking the intensity of the burst sensation when dissolved in water.

[0082] Furthermore, based on the insufficient compositional uniformity observed with mixtures containing gas-filled crystals having a particle size greater than 0.85 mm (Figure 13), and the improved mixing uniformity with mixtures containing gas-filled crystals having a particle size less than 0.85 mm (Figure 14), relatively small gas-filled crystals exhibit superior physical properties that make them more suitable for nutrition, health, and pharmaceutical products. Example 5 Official Exam

[0083] A comparative test of cumulative rupture signals for gas-filled crystals with various particle size ranges described in Example 4 was performed on commercially available Pop Rocks and ICEE popping candy using the method described in Example 3. In this experiment, the microphone used was a GRAS146AE from GRAS Sound & Vibration, and the audio analyzer was an Apx517B from Audio Precision.

[0084] Three samples of gas-filled crystals with different particle size ranges were prepared: Sample 1 was 0.546 mm to 0.66 mm, Sample 2 was 0.6 mm to 0.85 mm, and Sample 3 was 0.85 mm to 1.00 mm. In addition, commercially available Pop Rocks popping candy (Sample 4) and ICEE popping candy (Sample 5) were obtained and prepared. Nine replicates of Samples 1 and 2 were prepared and tested, eight replicates of Sample 3 were prepared and tested, seven replicates of Sample 4 were prepared and tested, and nine replicates of Sample 5 were prepared and tested. According to Example 4, each replicate of Samples 1-5 was approximately 250 mg. To account for some variation caused by ambient conditions, testing was performed by testing batches of two or three replicates daily over three days.

[0085] The methods described in Examples 3 and 4 were repeated with respect to Example 5, but there were two notable differences. First, as previously discussed herein, the average particle size in Pop Rocks and ICEE was considerably larger, exceeding 1 mm in diameter, and often as large as 4 mm in diameter. This means that larger crystals take longer to dissolve, resulting in a relatively longer time for the popping sensation to occur. To account for this, the length of the audio recording for each iteration was increased from 10 minutes to 20 minutes to allow all popping sensations to occur. Second, due to stronger signals from the Pop Rocks and ICEE samples, the voltage input range was increased from 0.8 V to 2.5 V. None of these changes were observed to produce inconsistent or contradictory results compared to the results in Example 4 and Figure 15, and the data were consistent for samples 1-3 in both Examples 4 and 5 and in Figures 15 and 16.

[0086] Figure 16 shows the signal area (Pa) for each of samples 1 to 5. rms * The graph shows the pressure over 10 seconds. As shown, for both sample 1, which has gas-filled crystals with a particle size of 0.546 mm to 0.66 mm, and sample 2, which has gas-filled crystals with a particle size of 0.6 mm to 0.85 mm, both were subjected to 0.6 Pa over 10 minutes. rms * The cumulative burst signal was less than 10 seconds, which is consistent with the results described in Example 4 and Figure 15. For sample 3, which has gas-filled crystals with a particle size of 0.85 mm to 1.00 mm, the cumulative burst signal was 0.6 Pa over 10 minutes. rms * It was observed that the time was over a second, which is also consistent with the results described in Example 4 and Figure 15.

[0087] For both Sample 4 (Pop Rocks) and Sample 5 (ICEE), the pressure was 0.6 Pa over 20 minutes. rms *The cumulative rupture signal exceeded 2 seconds. As shown in Figure 16, the cumulative rupture signal for each repeat varied significantly, by approximately 0.8 Pa. rms * From the cumulative rupture signal in seconds, up to approximately 3.6+ Pa rms * The range was up to seconds. The large variability is thought to be due to the relatively large gas-filled crystal grain size and the lack of uniformity in grain size between samples. Additionally, the dramatic increase and variability in the bursting intensity of Pop Rocks and ICEE commercial products upon dissolution with water is consistent with negative consumer feedback.

Claims

1. A gas-filled crystal having a particle size of 0.2 mm to 0.85 mm, wherein a 250 mg sample of the gas-filled crystal dissolves in water for 10 minutes, with a maximum pressure of 0.6 Pa. rms * The gas-filled crystal that generates a cumulative burst signal over seconds. A composition containing the following:

2. Cumulative rupture signal is 0.2–0.6 Pa rms * The composition according to claim 1, which is in seconds.

3. Gas-filled crystals: sugars; and Pressurized gas sealed in cavities within gas-filled crystals The composition according to claim 1, comprising:

4. The composition according to claim 3, wherein the sugar comprises glucose, fructose, sucrose, lactose, maltose, corn syrup, glucose syrup, or any combination thereof.

5. The composition according to claim 3, wherein the sugars include sucrose and glucose syrup.

6. The composition according to any one of claims 3 to 5, wherein the gas-filled crystals further contain an acidulant.

7. The composition according to claim 6, wherein the acidulant is malic acid.

8. The composition according to any one of claims 3 to 5, wherein the gas comprises carbon dioxide, nitrogen, air, a noble gas, or a combination thereof.

9. The composition according to any one of claims 3 to 5, wherein the pressurized gas has a pressure greater than 1 atmosphere.

10. The composition according to any one of claims 1 to 5, further comprising one or more vitamins, minerals, biological activators, active pharmaceutical ingredients, or any combination thereof.

11. The composition according to claim 10, wherein the vitamins include vitamin A, vitamin B (including B3, B6, B9, B12, and biotin), vitamin C, vitamin D, vitamin E, vitamin K, thiamine, riboflavin, niacin, folic acid, pantothenic acid, pharmaceutically acceptable salts thereof, or combinations thereof.

12. The composition according to claim 10, wherein the minerals include iron, phosphorus, iodine, copper, chromium, molybdenum, chloride, sodium, magnesium, calcium, zinc, selenium, manganese, potassium, choline, silicon, pharmaceutically acceptable salts thereof, or any combination thereof.

13. The composition according to claim 10, wherein the biological activator comprises lycopene, lutein, L-threonine, coenzyme Q-10, plant sterols, hyaluronic acid, cognitive citicoline, nicotinamide, andrographis, or any combination thereof.

14. The composition according to claim 10, wherein the active pharmaceutical ingredient comprises an analgesic or anti-inflammatory agent, an antihistamine, a decongestant, an antitussive, a biological activator, a sleep aid, a stress-reducing aid, an energy and cognitive aid, an Ayurvedic supplement, an immune supplement, a digestive aid, a joint supplement, a cannabinoid, a systemic natural substance, a nutritional supplement, a pharmaceutically acceptable salt thereof, or a combination thereof.

15. The composition according to any one of claims 1 to 5, further comprising a sweetener.

16. The composition according to claim 15, wherein the sweetener comprises glucose, fructose, sucrose, lactose, maltose, corn syrup, or any combination thereof.

17. The composition according to any one of claims 1 to 5, further comprising a diluent, a flavoring agent, a coloring agent, a preservative, or a combination thereof.

18. The composition according to any one of claims 1 to 5, wherein the gas-filled crystals have a particle size of 0.5 to 0.7 mm.

19. Gas-filled crystals with a particle size of 0.25–0.85 mm, containing sucrose, glucose syrup, and pressurized gas sealed in cavities within the gas-filled crystals. A composition comprising a 250 mg sample of gas-filled crystals, which dissolves in water for 10 minutes and exhibits a reaction of 0.2 to 0.6 Pa rms * The composition that produces a burst signal in seconds.

20. The composition according to claim 19, wherein the gas is carbon dioxide pressurized to more than 1 atmosphere.

21. The composition according to claim 19, further comprising one or more vitamins, minerals, biological activators, active pharmaceutical ingredients, or any combination thereof.

22. The composition according to any one of claims 19 to 21, further comprising an acidulant.

23. The composition according to claim 22, wherein the acidulant is malic acid.

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