Sweetener compound
By incorporating a high ratio of amorphous silica particles within sweetener formulations, the formulations enhance sweetness and reduce sweetener usage, addressing dissolution rate and cost issues in sweetener products.
Patent Information
- Application Number
- JP2025546199
- Authority / Receiving Office
- JP · JP
- Patent Type
- Applications
- Current Assignee / Owner
- Priority Date
- 2023-02-09
- Filing Date
- 2024-02-09
- Publication Date
- 2026-02-13
AI Technical Summary
Existing sweetener formulations containing amorphous silica particles exhibit reduced dissolution rates and perceived sweetness, leading to potential sweetness deficiencies and increased production costs.
Formulations incorporating a high ratio of amorphous silica particles within sweetener particles, where the sweetener particles are coated with a silica layer, enhance sweetness when diluted with conventional sweeteners, allowing for reduced sweetener usage without compromising taste.
The formulations achieve improved sweetness perception and lower production costs by utilizing less caloric sweeteners, maintaining texture and taste comparable to conventional products.
Smart Images

Figure 2026505403000001_ABST
Abstract
Description
[Background technology]
[0001] The present invention relates to sweet formulations containing silica within sweetener particles. Summary of the Invention
[0002] In accordance with the teachings of the present invention, a formulation is provided comprising a first population of sweetener particles, each individual sweetener particle comprising a caloric sweetener and a plurality of amorphous silica particles disposed within each individual sweetener particle, wherein the average ratio of the number of amorphous silica particles to the number of sweetener particles is at least 2.5:1, the first population of sweetener particles is less sweet than a control sweetener identical to the first population of sweetener particles but lacking the plurality of amorphous silica particles, and when the first population is diluted with sucrose to produce a standard formulation containing 0.1% amorphous silica, the standard formulation exhibits an improved sweetness relative to a corresponding control sucrose formulation identical to the standard formulation but lacking the plurality of amorphous silica particles.
[0003] Additional aspects and embodiments of the present invention will become apparent from the detailed description provided below.
[0004] The present invention will now be described, by way of example only, with reference to the accompanying drawings. While the description will now be made with specific and detailed reference to the drawings, it is emphasized that the detailed description is merely exemplary and is intended to illustrate preferred embodiments of the invention, presented in the course of providing what is believed to be the most useful and readily understandable explanation of the principles and conceptual aspects of the invention. In this regard, only those structural details of the invention necessary for a fundamental understanding of the invention have been shown, but, taken together with the drawings, it will become apparent to those skilled in the art how several forms of the invention may be embodied in practice. [Brief explanation of the drawings]
[0005] [Figure 1]FIG. 1 is a block diagram of a method for producing silica-and-sweetener particles according to an embodiment of the present invention. [Figure 2] FIG. 2 is a schematic diagram of a slurry of sweetener particles and silica particles disposed in a concentrated sweetener solution, according to an embodiment of the method of the present invention. [Figure 3] FIG. 1 is a schematic diagram of an exemplary crystallizer for performing step 104, according to an embodiment of the method of the present invention. [Figure 4] 1 is a schematic diagram of a silica-and-sweetener coated sweetener particle (e.g., coated sugar particle) according to an embodiment of the present invention. [Figure 5] 1 is a schematic diagram of a silica-and-sweetener coated sweetener particle consisting of a core having a radius or characteristic radius R, the core being covered or at least partially covered by a shell. [Figure 6A] 1 is a graph showing the dissolution rate of sucrose formulations containing low concentrations of amorphous silica compared to a crystalline sucrose control formulation. [Figure 6B] 1 is a graph showing the dissolution rate of a sucrose sweetener concentrate according to the present invention compared to a crystalline sucrose control formulation. [Figure 7] 1 provides X-ray diffraction (XRD) plots illustrating the crystalline characteristics of various sweetener-and-silica sweetener concentrate formulations according to embodiments of the present invention. [Figure 8] FIG. 1 is an enlarged schematic diagram of a sweetener formulation containing silica- and sweetener-coated sweetener particles diluted with conventional sweetener particles, according to an embodiment of the present invention. [Figure 9] Photographs of muffins of the present invention versus two control muffins. DETAILED DESCRIPTION OF THE INVENTION
[0006] The present disclosure describes improved sweetener formulations and methods for making such improved sweetener formulations and for utilizing them in food products.
[0007] The present disclosure describes sweetener-and-silica sweetener compositions and methods for making such compositions and using them in food products. In some embodiments, the compositions may include a sweetener kernel containing at least one of a sweetener carbohydrate (e.g., sucrose) and a sweetener polyol. The coating surrounding the kernel includes amorphous silica and a sweetener, typically a sugar.
[0008] The use of amorphous silica to enhance the sweetness of sugars is known, with the amorphous silica acting as a carrier for the sugars which are formed as amorphous sugars on the surface of the amorphous silica.
[0009] In water, amorphous sugars are known to have an improved dissolution rate relative to crystalline sugars: during eating, the amount of sugar that dissolves in the mouth is higher for amorphous sugars relative to their crystalline counterparts.
[0010] The sweetener- and silica sweetener particles in the compositions of the present invention exhibit dissolution rates that can be disadvantageously significantly lower than the dissolution rates of the corresponding amorphous sweeteners, and may even exhibit dissolution rates significantly lower than the dissolution rates of the corresponding fully crystalline sweeteners.
[0011] Not surprisingly, the perceived sweetness of such sweetener-and-silica sweetener particles can be significantly reduced relative to a control sweetener formulation identical to the sweetener formulation but lacking amorphous silica.
[0012] Despite this deficiency, the inventors have surprisingly discovered that when placed in a formulation containing one or more types of conventional sweetener particles (e.g., table sugar), such compromised sweetener-and-silica sweetener particles can actually enhance the overall perceived sweetness of the formulation. For example, when the sweetener-and-silica sweetener particles are "diluted" with table sugar and utilized in a food product such as a confectionery or sweet baked good (cake, cookie, pastry, etc.), the food product can exhibit significantly improved sweetness relative to a control food product having the same concentration of sweetener (in this example, conventional sugar) but lacking amorphous silica.
[0013] Alternatively, the food products of the present invention can be formulated to contain significantly less caloric sweetener (e.g., 20% to 50% less) than corresponding conventional food products without a reduction in perceived sweetness.
[0014] In addition to the obvious health benefits, the use of sweetener-and-silica sweetener particles with compromised sweetness diluted with conventional sweeteners, such as conventional crystalline sugar, can lead to significantly lower production costs for various food products relative to sweetener-and-silica sweetener formulations in which essentially all of the sweetener particles contain silica at low concentrations.
[0015] Referring now to the figures, Figure 1 is a block diagram of a method for producing silica- and sweetener-containing particles according to an embodiment of the present invention. Step 102 of the method includes providing a slurry containing solids, including silica particles and sweetener kernel particles, such as sucrose, disposed in an aqueous medium containing a dissolved sweetener.
[0016] In some embodiments, step 102 of the method may include contacting sweetener particles with an aqueous medium containing dissolved sweetener and silica particles to produce a slurry containing sweetener kernel particles and silica particles in a sweetener solution ("concentrated sweetener solution" or "concentrated sugar solution").
[0017] 2 provides a schematic diagram of such a slurry 200, in which sweetener kernel particles 202 and silica particles 204 are in contact with an aqueous sweetener solution 206. It will be understood that the aqueous sweetener solution 206 can be saturated or substantially saturated with respect to the sweetener.
[0018] Typically, the sweetener is a sugar such as sucrose, however, in the general process description provided below, the term "sugar" is meant to refer to the more general case, i.e., "caloric sweetener."
[0019] As used herein, the term "caloric sweetener" refers to at least one sweetener selected from the group consisting of sweetener carbohydrates (e.g., sucrose) and sweetener polyols (e.g., maltitol).
[0020] Step 104 of the method may include depositing at least a portion of the sweetener dissolved in the aqueous medium onto the sweetener kernel particles to produce a sweetener coating over the sweetener kernel particles, the sweetener coating including at least a portion of the silica particles. Step 104 is optional and may be performed in a crystallizer, such as a cooling crystallizer, a flash cooling crystallizer, or an evaporative crystallizer. Forced circulation crystallizers, draft tube crystallizers, Oslo crystallizers, and other types of crystallizers may be used. Supersaturation with respect to the sweetener may result in precipitation of the sweetener as crystals (e.g., by secondary nucleation) and / or on the surface of the amorphous silica.
[0021] Step 106 of the method optionally includes separating the first portion of the aqueous medium (e.g., from step 102 or step 104) and the first portion of the silica particles from the sugar kernel particles. As a result, a wet cake may be produced in which the second portion of the aqueous medium and the second portion of the silica particles may be disposed around the sugar kernel particles.
[0022] Method step 108 optionally includes drying at least a portion of the sweetener product or at least a portion of the solids (e.g., from any of steps 102, 104, and / or 106) to produce a dried sweetener product ("silica and sweetener concentrate") containing a high concentration of amorphous silica. This concentrate may also contain coated sweetener particles having a silica-and-sweetener coating over the sweetener kernel particles. The sugar-and-silica coating may include silica particles from the second portion of the silica particles.
[0023] Both batch and continuous processes can be utilized in the methods of the present invention.
[0024] FIG. 3 is a schematic diagram of an exemplary crystallizer for performing step 104 according to an embodiment of the method of the present invention.
[0025] 4 is a schematic diagram of a coated sweetener particle according to an embodiment of the present invention. In this embodiment, the coated sweetener particle has a radius or characteristic radius R カーネル and the core consists of a central kernel having a characteristic thickness T コーティング The kernel is typically covered or at least partially covered by a coating having a silica concentration of 0.01% by weight, where 0.01% by weight is the average silica concentration in the coating. SILコーティング is the average weight concentration of silica in the kernel, C SILカーネル It is clear that: C SILコーティング> C SILカーネル
[0026] Ratio C SILカーネル / C SILコーティング can be at most 0.2, more typically at most 0.1, at most 0.05, or at most 0.02. Most typically, C SILカーネル / C SILコーティング can be 0 or substantially 0.
[0027] It will be understood by those skilled in the art that a variety of analytical techniques may be used to characterize the outer layer or coating of the coated sweetener particles and compare its properties to those of the material underlying the coating.
[0028] In some embodiments, the silica utilized in accordance with the present invention is amorphous silica having an average particle size (Dv50-S) in the range of 0.8 to 20 micrometers (μm).
[0029] In some embodiments, the DV50-S is at least 1.5 mm, at least 2 mm, at least 2.5 mm, or at least 3 mm, at least 5 mm, at least 6 mm, or at least 7 mm.
[0030] In some embodiments, the DV50-S is at most 18 mm, at most 16 mm, at most 14 mm, or at most 12 mm.
[0031] In some embodiments, DV50-S is within the range of 1.5 to 20 mm, 2 to 20 mm, 3 to 20 mm, 4 to 20 mm, 5 to 20 mm, 6 to 20 mm, 7 to 20 mm, 1.5 to 15 mm, 2.5 to 15 mm, or 3 to 15 mm.
[0032] Referring now to FIG. 5, FIG. 5 shows a radius or characteristic radius R コア 1 is a schematic diagram of a spherical sweetener particle consisting of a core having a thickness T シェル The core is covered or at least partially covered by a shell having a thickness of 1000 Å. As described above, an etching process (such as that described in Example 26 below) can be performed to remove a portion of the shell without dissolving any (or very little) of the core. Alternatively, the etching process can be designed to remove substantially all of the shell while dissolving only a portion or a relatively small portion of the core.
[0033] As used herein and in the claims, the term "standard etching process" refers to an etching process that removes, on average, 10 micrometers of coated sweetener particles. The value of 10 micrometers is calculated based on a spherical model of the particles, as shown in Figure 5. This model further assumes that the sweetener particles are all D V Assume that the particles have a size of 50 and the particle volume is the average size of the population.
[0034] Because the kernel is typically pure sugar or sweetener, the "core" may be devoid (i.e., typically devoid) or substantially devoid of silica. The average (weight) concentration of silica in the coating, C SILシェル is the average (weight) concentration of silica in the core, C SILコア It is clear that: C SILシェル> C SILコア
[0035] Ratio C SILシェル> C SILコア can be at most 0.2, more typically at most 0.1, at most 0.05, or at most 0.02. Most typically, C SILシェル> C SILコア may be 0 or substantially 0. As above, these concentrations are calculated on a sweetener plus silica basis.
[0036] It will be understood by those skilled in the art that a variety of analytical techniques can be used to characterize the outer shell of coated sweetener particles and compare the properties to the properties of the material in the core underlying the coating.
[0037] 6A is a graph showing the dissolution rate of a sucrose formulation containing a low concentration of amorphous silica compared to a corresponding crystalline sucrose control formulation. The concentration of dissolved sweetener (sucrose) is plotted as a function of dissolution time. The experimental conditions are provided in Example 94 below.
[0038] It is clear from Figure 6A that pure crystalline sucrose exhibited the slowest dissolution rate. All three of the sucrose samples containing amorphous silica exhibited faster dissolution rates, with the rate increasing monotonically with increasing amorphous silica concentration. After 30 seconds, which may be the most critical period for foods that are chewed and savored, the dissolution rate of the sample containing 1% amorphous silica exceeded that of the pure crystalline sucrose sample by more than 25%.
[0039] 6B is a graph showing the dissolution rate of a sweetener concentrate according to the present invention containing 50% sucrose and 50% amorphous silica compared to a corresponding crystalline control formulation. The concentration of dissolved sweetener (sucrose) is plotted as a function of dissolution time. The experimental conditions are provided in Example 95 below.
[0040] It is clear from Figure 6B that the sweetener concentrates according to the present invention exhibit significantly slower dissolution rates than the sucrose control formulation. This is surprising given that the sucrose control formulation is entirely crystalline. It is even more surprising in light of the results shown in Figure 6A, where all of the sweetener concentrates containing amorphous silica achieve faster dissolution rates relative to the same sucrose control formulation utilized in Example 95.
[0041] 7 provides X-ray diffraction (XRD) plots showing the crystalline characteristics of various sweetener- and silica-sweetener concentrate formulations according to embodiments of the present invention. From the XRD plots, it is clear that various sweetener (sucrose) samples are crystalline or exhibit crystalline behavior even at relatively high concentrations of amorphous silica. The inventors have found that such crystalline behavior can be observed at amorphous silica concentrations of up to 50% or more.
[0042] FIG. 8 is an enlarged schematic diagram of a sweetener formulation 600 containing silica-and-sweetener coated sweetener particles 602 diluted with or mixed with sweetener particles 604, such as conventional sweetener particles (e.g., crystalline sucrose), according to an embodiment of the present invention.
[0043] This advantageously allows for the use of ordinary, conventional, inexpensive sweetener materials (e.g., crystalline sucrose products such as table sugar) as the primary component of the sweetener formulation of the present invention. For example, in a diluted sweetener formulation using a caloric sweetener concentrate with a final silica concentration of 0.2% and containing 50% caloric sweetener and 50% amorphous silica, 1 ton of the diluted formulation of the present invention requires 2 kg of amorphous silica (i.e., 4 kg of sweetener concentrate), resulting in a requirement of 996 kg of a typical sweetener, such as table sugar. For a second example, in a diluted sweetener formulation using a caloric sweetener concentrate with a final silica concentration of 0.4% and containing 84% caloric sweetener and 16% amorphous silica, 1 ton of the diluted formulation of the present invention requires 4 kg of amorphous silica (i.e., 25 kg of sweetener concentrate [100% / 16%] x 4), resulting in a requirement of 975 kg of a typical sweetener, such as table sugar.
[0044] The concentration of amorphous silica in diluted sweetener formulations is typically 0.05% to 2%. The concentration of amorphous silica in food products (e.g., confectionery, sweet baked goods, etc.) is typically 0.003% to 1%.
[0045] Figure 9 is a photograph comparing a muffin of the present invention with two control muffins. The muffins on the left ("Invention Formulation") and right ("Control II") were prepared according to Examples 82 and 82A, provided below. The muffin in the middle ("Control I") contained the same silica-and-sugar concentrate as the invention formulation and the same concentration of sugar as the invention formulation. However, instead of being diluted with regular sugar as in the invention formulation, all of the sugar was provided by the silica-and-sugar concentrate.
[0046] The texture of the muffins of the present invention has been found to be advantageously similar to the excellent texture of conventional all-sugar (crystalline sucrose) muffins.
[0047] With regard to the sweetness of the muffins, the Control I muffins containing undiluted silica-sucrose concentrate (approximately 40% sugar reduction) were found to be significantly less sweet than both the full sugar Control II muffins, which were found to be of comparable sweetness, and the inventive muffins containing diluted silica-sucrose concentrate (approximately 40% sugar reduction). [Example]
[0048] Reference is now made to the following examples, which together with the above descriptions, illustrate the invention in a non limiting sense. List of equipment used: [Table 1] List of materials used: [Table 2]
[0049] Example 1 A concentrated sugar syrup, typically containing about 60-75% sugar by weight, is typically prepared in a Thermomix® cooker mixer at approximately 60°C-70°C. The solution density, in Brix, may be measured using an ATAGO® pocket refractometer. Sugar is then gradually added under constant mixing to produce a slurry containing sugar particles. The sugar may be pre-classified (e.g., by sieving) to obtain a specific fraction or size distribution. Food-grade amorphous silica is then gradually added under constant mixing to produce a slurry of sugar and silica particles in a substantially saturated sugar solution.
[0050] Example 2 Sugar is added to water (or an unsaturated sugar solution) in a Thermomix® cooker mixer under constant mixing to produce a concentrated sugar solution or sugar slurry that can be substantially saturated with sugar (typically containing 90% to 95% of the amount of sugar needed to achieve saturation at that particular temperature). Alternatively, a substantially saturated solution is produced by adding sugar in 15% to 30% excess over the amount needed to achieve saturation at the target temperature. After one hour of mixing, a solid / liquid separation is performed (typically in a heated filtration unit) to separate the excess sugar solids, leaving a clear, substantially saturated solution. Food-grade amorphous silica is gradually added under constant mixing. Sugar is then gradually added under constant mixing to produce a slurry containing sugar particles and amorphous silica. The sugar may be pre-classified (e.g., by sieving) to obtain a specific fraction or size distribution for incorporation into the syrup. Typically, the temperature of the crystallizer contents is maintained at 60°C.
[0051] Example 3 Sugar is added to water in a Thermomix® cooker mixer under constant mixing to produce a solution that is substantially saturated with sugar. Food-grade amorphous silica may be added incrementally to the water or sugar solution under constant mixing. The addition of silica may be before, simultaneously with, or at least partially simultaneous with the addition of sugar. Sugar is gradually added to the sugar solution containing silica under constant mixing to produce a slurry containing sugar particles and silica. The sugar may be pre-classified (e.g., by sieving) to obtain a particular fraction or size distribution.
[0052] Example 4: Cooling crystallization to produce coated sugar kernel particles A crystallizer is charged with a slurry containing sugar and food-grade amorphous silica in a concentrated syrup of sugar, for example, prepared according to any of Examples 1-3, and the slurry is maintained at a temperature within the range of 60-80°C under constant mixing using an IKA high shear mixer. The crystallizer is then cooled, typically to 25-45°C, by means of a heat transfer fluid placed within the crystallizer jacket. During cooling, which usually takes about 2 hours, the saturation concentration of the sugar decreases and supersaturation results in a coating of sugar and silica on the pure sugar kernel.
[0053] Example 5: Evaporative cooling crystallization to produce coated sugar kernel particles A crystallizer is charged with a slurry containing sugar and amorphous silica in a concentrated sugar syrup, for example, prepared according to any of Examples 1-3, and the slurry is maintained at a temperature within the range of 60-80°C under constant mixing for approximately 20 minutes using an IKA high shear mixer. The crystallizer is then cooled to 25-45°C, and a vacuum is applied to maintain the crystallizer at this temperature. During cooling, which typically takes approximately 2 hours, the sugar saturation concentration decreases, and supersaturation results in a coating of sugar and silica on the pure sugar kernels. It will be appreciated that a higher initial temperature of the slurry and / or a lower cooling temperature within the crystallizer will increase the kernel to coating weight ratio.
[0054] Example 6: Evaporative crystallization to produce coated sugar kernel particles A crystallizer is charged with a slurry containing sugar and amorphous silica in a concentrated sugar syrup, for example, prepared according to any of Examples 1-3, and the slurry is maintained at a temperature within the range of 60-80°C under constant mixing for about 20 minutes using an IKA high shear mixer. A vacuum is then applied to evaporate water from the system while maintaining the temperature within the range of 60-80°C. The resulting supersaturation results in a coating of sugar and silica on the pure sugar kernels.
[0055] Example 7: Solid / Liquid Separation Following crystallization (per any of Steps 4-6), the slurry is immediately transferred to a filtration device, such as a belt filter or a centrifuge (e.g., MRC Model BK-30), typically operated at room temperature. The centrifuge separates the filtrate from the coated sugar, resulting in a moist sugar cake containing the coated sugar particles. The centrifugation time can be varied to obtain a given or desired level of moisture, with it being understood that higher centrifugation times (and / or higher centrifugal forces) are associated with lower ratios of coating weight to kernel weight or coating thickness to kernel size (radius or diameter).
[0056] Example 8: Solid / Liquid Separation Following production of a slurry containing sugar and amorphous silica particles in a concentrated solution of sugar (according to any of Examples 1-3), the slurry is immediately transferred to a filtration device, such as a belt filter or centrifuge (e.g., MRC Model BK-30), typically operating at room temperature. The filtration device separates the filtrate from the sugar particles, resulting in a moist sugar cake containing the sugar particles (surrounded by a layer of mother liquor). It will be understood that the filtration or centrifugation time can be varied to obtain a given or desired level of moisture, with higher centrifugation times (and / or higher centrifugal forces) being associated with lower ratios of coating weight to kernel weight or coating thickness to kernel size.
[0057] Example 8A: Preparation of a dry coated sugar powder The coated sugar produced (e.g., by the method of Example 7 or Example 8) can be transferred to a fluidized bed dryer (Retsch® TG100). The drying program is typically as follows: 2 minutes at temperature 4 with blower at level 3, 2 minutes at temperature 5 with blower at level 4, and 2 minutes at temperature 6 with blower at level 4.
[0058] Example 9 A sweetener syrup containing one or more carbohydrate sweeteners and / or one or more polyol (typically sugar alcohol) sweeteners is prepared before the addition of silica. The temperature of the sweetener syrup is generally maintained within a range of 25°C to, in some cases, approximately 80°C. For sucrose, the default temperature is 60°C. The sweetener-to-water concentration is typically within the range of 1% to 65% by weight for most carbohydrate and polyol sweeteners (and may depend on the ratio of silica to sweetener). Some sweeteners with lower solubility may require relatively high water concentrations and / or elevated temperatures to fully dissolve. Silica is then gradually added under constant mixing. Once the silica addition is complete, the mixing vessel is continued to be agitated using a high-shear mixer for at least 7 minutes until the silica is completely dispersed within the sweetener syrup.
[0059] Example 9A The silica-sweetener concentrate syrup (e.g., produced according to Example 9) can be transferred to a heated double-jacketed vessel in a vacuum dryer (e.g., Stephan). The vessel is heated (typically 60°C to 70°C), maintained under vacuum, and constantly mixed to evaporate water, preferably at a slow, controlled rate, to achieve low levels of global and local supersaturation within the stirred vessel. Finally, a silica-sweetener concentrate powder is produced. Typically, the powder is crystalline or exhibits distinct crystalline behavior that can be observed under an optical microscope and / or identified and quantified by XRD.
[0060] Optionally, the powder may be transferred to an oven (typically operating at 65° C.) for further drying for several hours or overnight.
[0061] Example 9B The silica-sweetener concentrate is typically in powder form and may optionally be subjected to size reduction. The silica-sweetener powder is milled to a D sieve size, typically in the range of 20 to 300 micrometers. 50 A fine powder having
[0062] Example 10 The silica-sweetener concentrate (e.g., produced by Example 8A or Example 9A) is diluted with at least one normal calorie sweetener (carbohydrate sweetener) and / or at least one polyol (typically a sugar alcohol) sweetener to achieve the desired amount of silica in the sweetener formulation. For example, to prepare a "diluted" silica sweetener formulation or a "full-strength silica sweetener" formulation containing an average of 0.3% silica from a silica-sweetener concentrate containing 50% silica, 0.6 grams of the silica-sweetener concentrate formulation is mixed with 99.4 grams of a normal carbohydrate sweetener (e.g., sucrose) and / or polyol sweetener.
[0063] Silica-sweetener concentrates are D 50 or D within this range 50 can be subjected to size reduction to obtain
[0064] Example 11A: Use of Sweetener Ingredients in the Formulation of Edible Formulations A "diluted" or "full strength" silica sweetener formulation (e.g., produced according to Example 10), which may be a mixture of silica-sweetener concentrate and regular sweetener, can be added as an ingredient along with other ingredients, mixed, and optionally further processed (e.g., baked) to produce an edible formulation (e.g., cakes, muffins, biscuits).
[0065] Example 11B Another way to utilize the silica-sweetener concentrate formulation is to add the required amount of silica-sweetener concentrate—as a separate ingredient—to a regular sweetener (carbohydrate sweetener and / or polyol sweetener) during the preparation of an edible formulation (e.g., muffin). For example, to obtain a sweetener having an average silica concentration of 0.3% from a regular sweetener and a concentrated silica-containing sweetener containing 50% silica in an edible formulation, 0.6 grams of silica-sweetener concentrate is added together with 99.4 grams of regular sweetener. Thus, the silica-sweetener concentrate and regular sweetener can be added as separate ingredients, rather than as a mixture.
[0066] Example 12 A concentrated sugar syrup was prepared by mixing 726 g of Sugat® sugar (food-grade sucrose) with 210 g of water at 60°C, followed by filtration according to Example 2 to produce a substantially saturated sugar solution containing approximately 605 g of sugar. An additional amount of sugar was sieved to obtain the 500-600 μm fraction, with the other fractions discarded. 600 g of the sieved sugar (approximately the 500-600 μm fraction) was gradually added to the crystallizer over several minutes under constant mixing. Subsequently, 6.0 g of silica (Syloid® 9005PC) was gradually added over 30 seconds, again under constant mixing. This amount represents 0.5% by weight of pure silica relative to the total amount of sugar in the process (i.e., in the syrup + sieved sugar).
[0067] Cooling crystallization was then carried out according to the procedure described in Example 4. The initial temperature of the slurry was about 70°C. The crystallizer was cooled to about 30°C by means of a heat transfer fluid placed in the crystallizer jacket, producing coated sugar kernel particles. Solid / liquid separation was carried out according to Example 7 with a centrifugation time of 40 seconds. Drying of the silica- and sugar-coated sugar was carried out by means of a fluidized bed dryer according to the procedure provided in Example 8A. The concentration of pure silica relative to the concentration of sugar in the coated sugar particles was approximately 0.14%.
[0068] Example 13 A concentrated sugar syrup was prepared at 60°C according to Example 12. An additional amount of sugar was sieved to obtain the 500-600 μm fraction, and the other fractions were discarded. 600 g of sieved sugar (500-600 μm fraction) was gradually added to the crystallizer over 1 minute under constant mixing. Subsequently, 3.0 g of silica (Syloid® 9005) was gradually added over 30 seconds, again under constant mixing. This amount represented 0.25% by weight of pure silica relative to the total amount of sugar in the process (i.e., in the syrup + sieved sugar).
[0069] Cooling crystallization was then carried out according to the procedure described in Example 4. The initial temperature of the slurry was about 60°C. The crystallizer was cooled to about 30°C by means of a heat transfer fluid placed in the jacket of the crystallizer, producing coated sugar kernel particles. Solid / liquid separation was carried out according to Example 7 with a centrifugation time of 40 seconds. Drying of the silica- and sugar-coated sugar was carried out by means of a fluidized bed dryer according to the procedure provided in Example 8A. The concentration of pure silica relative to the concentration of sugar in the coated sugar particles was approximately 0.06%.
[0070] Example 14 A concentrated sugar syrup was prepared at 60°C according to Example 12. An additional amount of sugar was sieved to obtain the 500-600 μm fraction, and the other fractions were discarded. 600 g of sieved sugar (500-600 μm fraction) was gradually added to the crystallizer over 1 minute under constant mixing. Subsequently, 6.0 g of silica (T-700) was gradually added over 30 seconds, again under constant mixing. This amount represented 0.5% by weight of pure silica relative to the total amount of sugar in the process (i.e., in the syrup + sieved sugar).
[0071] Evaporative cooling crystallization was then carried out according to the procedure described in Example 5. The initial temperature of the slurry was about 60°C. The crystallizer was cooled to about 30°C, and coated sugar kernel particles were produced by means of vacuum. Solid / liquid separation was carried out according to Example 7 with a centrifugation time of 40 seconds. Drying of the silica- and sugar-coated sugar was carried out by means of a fluidized bed dryer according to the procedure provided in Example 8A.
[0072] The dried silica- and sugar-coated sugar product weighed 729 g, representing a 124 g (729 g - 605 g) or 20.5% increase relative to the weight of the sugar kernels and a 17% increase relative to the weight of the entire coated sugar particle (124 g / 729 g). The silica content of the dried silica- and sugar-coated sugar product was 1.2 grams, all of which was disposed in the coating. Thus, the average silica concentration in the coating was 1.2 g / 124 g, or approximately 1.0%, and the average silica:sugar weight ratio in the coating was 1.2 g / 122.8 g, or approximately 0.01. The average silica concentration relative to the sugar concentration in the entire coated sugar particle was 1.2 g / 729 g, or approximately 0.16%, and the average silica:sugar weight ratio in the entire coated sugar particle was 1.2 g / 727.8 g, or approximately 0.0016.
[0073] Example 15 A concentrated sugar syrup was prepared at 60°C according to Example 12. An additional amount of sugar was sieved to obtain the 500-600 μm fraction, and the other fractions were discarded. 600 g of sieved sugar (500-600 μm fraction) was gradually added to the crystallizer over a period of 1 minute under constant mixing. Subsequently, 2.0 g of silica (Syloid® 9005) was gradually added over a period of 30 seconds, again under constant mixing. This amount represents approximately 0.17% by weight of pure silica relative to the total amount of sugar in the process (i.e., in the syrup + sieved sugar).
[0074] Cooling crystallization was then carried out according to the procedure described in Example 4. The initial temperature of the slurry was about 70°C. The crystallizer was cooled to about 30°C by means of a heat transfer fluid placed in the jacket of the crystallizer, producing coated sugar kernel particles. Solid / liquid separation was carried out according to Example 7 with a centrifugation time of 40 seconds. Drying of the silica- and sugar-coated sugar was carried out by means of a fluidized bed dryer according to the procedure provided in Example 8A.
[0075] The weight of the coating consisting of sugar and sweetener was about 123 grams, or about 17% of the original weight of the sugar kernels. The amount of pure silica in the coating layer was 0.36 grams, corresponding to an average concentration (by weight) of silica relative to the sweetener (sugar) in the coating of about 0.29% of the coating (0.36 / 123). The concentration of pure silica relative to the concentration of sugar in the coated sugar particles, i.e., the average concentration (by weight) of silica relative to the sweetener (sugar), was 0.05%.
[0076] This was approximately equal to the average concentration (by weight) of silica in the coated particles, which was also about 0.05%.
[0077] The silica-and-sugar coated sugar was then diluted by adding Sugat® table sugar in a 1:1 ratio (Sugat®:coating sugar), which reduced the concentration of pure silica to 0.025% relative to the concentration of sugar in the sugar blend.
[0078] Example 16 A concentrated sugar syrup was prepared at 60°C according to Example 12. An additional amount of sugar was sieved to obtain the 500-600 μm fraction, and the other fractions were discarded. 600 g of sieved sugar (500-600 μm fraction) was gradually added to the crystallizer over a period of 1 minute under constant mixing. Subsequently, 4.0 g of silica (Flo-gard™ T-800) was gradually added over a period of 30 seconds, again under constant mixing. This amount represented 0.33% by weight of pure silica relative to the total amount of sugar in the process (i.e., in the syrup + sieved sugar).
[0079] Evaporative cooling crystallization was then carried out according to the procedure described in Example 5. The initial temperature of the slurry was about 60°C. The crystallizer was cooled to about 30°C, and coated sugar kernel particles were produced by means of vacuum. Solid / liquid separation was carried out according to Example 7 with a centrifugation time of 40 seconds. Drying of the silica- and sugar-coated sugar was carried out by means of a fluidized bed dryer according to the procedure provided in Example 8A. The concentration of pure silica relative to the concentration of sugar in the coated sugar particles was approximately 0.1%.
[0080] Example 17 A concentrated sugar syrup was prepared at 60°C according to Example 12. An additional amount of sugar was sieved to obtain the 500-600 μm fraction, and the other fractions were discarded. 600 g of the sieved sugar (500-600 μm fraction) was gradually added to the crystallizer over a period of 1 minute under constant mixing. Subsequently, 5.0 g of silica (Flo-gard™ 915) was gradually added over a period of 30 seconds, again under constant mixing. This amount represents approximately 0.41% by weight of pure silica relative to the total amount of sugar in the process (i.e., in the syrup + sieved sugar).
[0081] Cooling crystallization was then carried out according to the procedure described in Example 4. The initial temperature of the slurry was approximately 60°C. The crystallizer was cooled to approximately 30°C by means of a heat transfer fluid placed in the crystallizer jacket, producing silica- and sugar-coated sugar kernel particles. Solid / liquid separation was carried out according to Example 7 with a centrifugation time of 40 seconds. The silica- and sugar-coated sugar was dried by means of a fluidized bed dryer according to the procedure provided in Example 8A. The weight of the coating consisting of sugar and sweetener was approximately 138 grams, or approximately 23% of the initial weight of the sugar kernels. The amount of pure silica in the coating layer was approximately 0.72 grams, corresponding to an average concentration of approximately 0.52% by weight in the coating. The average concentration of pure silica relative to the average concentration of sugar in the coated sugar particles (i.e., average concentration based on silica relative to sugar) was approximately 0.1%.
[0082] The silica- and sugar-coated sugar was then diluted by a factor of 2 by adding Sugat® table sugar in a 1:1 ratio (Sugat®:coating sugar), which reduced the average concentration of pure silica to 0.05% relative to the average concentration of sugar in the sugar blend.
[0083] Example 18 A concentrated sugar syrup was prepared at 60°C according to Example 12. An additional amount of sugar was sieved to obtain the 500-600 μm fraction, and the other fractions were discarded. 600 g of sieved sugar (500-600 μm fraction) was gradually added to the crystallizer over a period of 1 minute under constant mixing. Subsequently, 20 g of silica (Flo-gard™ 915) was gradually added over a period of 30 seconds, again under constant mixing. This amount represented 1.66% by weight of pure silica relative to the total amount of sugar in the process (i.e., in the syrup + sieved sugar).
[0084] Cooling crystallization was then carried out according to the procedure described in Example 4. The initial temperature of the slurry was about 70°C. The crystallizer was cooled to about 30°C by means of a heat transfer fluid placed in the crystallizer jacket, producing silica- and sugar-coated sugar kernel particles. Solid / liquid separation was carried out according to Example 7 with a centrifugation time of 40 seconds. Drying of the silica- and sugar-coated sugar was carried out by means of a fluidized bed dryer according to the procedure provided in Example 8A. The weight of the coating was about 126 grams, or about 21% of the initial weight of the sugar kernels. The amount of pure silica in the coating layer was approximately 4.8 grams, corresponding to about 4.0% (silica:sugar) of the coating by weight. The average concentration of pure silica relative to the average concentration of sugar in the coated sugar particles (i.e., the average concentration based on silica to sugar) was about 0.66%.
[0085] The silica- and sugar-coated sugar was then diluted by a factor of 4 by adding Sugat® table sugar in a ratio of 3:1 (Sugat®:coating sugar), which reduced the average concentration of pure silica to 0.17% relative to the average concentration of sugar in the sugar blend.
[0086] Example 19 A concentrated sugar syrup was prepared at 60°C according to Example 12. An additional amount of sugar was sieved to obtain the 500-600 μm fraction, and the other fractions were discarded. 600 g of sieved sugar (500-600 μm fraction) was gradually added to the crystallizer over 1 minute under constant mixing. Subsequently, 1.5 g of silica (Flo-gard™ 233) was gradually added over 30 seconds, again under constant mixing. This amount represented 0.13% by weight of pure silica relative to the total amount of sugar in the process (i.e., in the syrup + sieved sugar).
[0087] Cooling crystallization was then carried out according to the procedure described in Example 4. The initial temperature of the slurry was about 70°C. The crystallizer was cooled to about 30°C by means of a heat transfer fluid placed in the jacket of the crystallizer, producing coated sugar kernel particles. Solid / liquid separation was carried out according to Example 7 with a centrifugation time of 40 seconds. Drying of the silica- and sugar-coated sugar was carried out by means of a fluidized bed dryer according to the procedure provided in Example 8A. The concentration of pure silica relative to the concentration of sugar in the coated sugar particles was approximately 0.04%.
[0088] Example 20 A concentrated sugar syrup was prepared at 60°C according to Example 12. An additional amount of sugar was sieved to obtain the 500-600 μm fraction, and the other fractions were discarded. 600 g of sieved sugar (500-600 μm fraction) was gradually added to the crystallizer over a period of 1 minute under constant mixing. Subsequently, 12 g of silica (Flo-gard™ T-700) was gradually added over a period of 30 seconds, again under constant mixing. This amount represents 1% by weight of pure silica relative to the total amount of sugar in the process (i.e., in the syrup + sieved sugar).
[0089] Evaporative cooling crystallization was then carried out according to the procedure described in Example 5. The initial temperature of the slurry was about 70°C. The crystallizer was cooled to about 30°C, and coated sugar kernel particles were produced by means of vacuum. Solid / liquid separation was carried out according to Example 7 with a centrifugation time of 40 seconds. The silica- and sugar-coated sugar was dried by means of a fluidized bed dryer according to the procedure provided in Example 8A. The weight of the coating was about 198 grams, or about 33% of the initial weight of the sugar kernels. The amount of pure silica in the coating layer was 3.99 grams, corresponding to an average concentration of about 2.0% in the coating. The concentration of pure silica relative to the concentration of sugar in the coated sugar particles (i.e., the average concentration based on silica relative to sugar) was 0.5%.
[0090] The silica- and sugar-coated sugar was then diluted by adding Sugat® table sugar in a ratio of 5.2:1 (Sugat®:coating sugar), which reduced the average concentration of pure silica to 0.08% relative to the average concentration of sugar in the sugar blend.
[0091] Example 21 A concentrated sugar syrup was prepared at 60°C according to Example 12. An additional amount of sugar was sieved to obtain the 500-600 μm fraction, and the other fractions were discarded. 600 g of sieved sugar (500-600 μm fraction) was gradually added to the crystallizer over 1 minute under constant mixing. Subsequently, 60 g of silica (Flo-gard™ T-700) was gradually added over 30 seconds, again under constant mixing. This amount represented 5% by weight of pure silica relative to the total amount of sugar in the process (i.e., in the syrup + sieved sugar).
[0092] Evaporative cooling crystallization was then carried out according to the procedure described in Example 5. The initial temperature of the slurry was about 60°C. The crystallizer was cooled to about 30°C, and coated sugar kernel particles were produced by means of vacuum. Solid / liquid separation was carried out according to Example 7 with a centrifugation time of 40 seconds. The silica- and sugar-coated sugar was dried by means of a fluidized bed dryer according to the procedure provided in Example 8A. The weight of the coating was about 108 grams, or about 18% of the initial weight of the sugar kernels. The amount of pure silica in the coating layer was approximately 11.9 grams, corresponding to an average concentration of about 11% of the coating. The average concentration of pure silica relative to the average concentration of sugar in the coated sugar particles (i.e., the average concentration based on silica relative to sugar) was approximately 1.71%, corresponding to an average silica concentration of about 1.68% in the coated particles.
[0093] The silica- and sugar-coated sugar was then diluted by a factor of 8.5 by adding Sugat® table sugar in a ratio of 7.5:1 (Sugat®:coating sugar), which reduced the average concentration of pure silica to 0.2% relative to the average concentration of sugar in the sugar blend.
[0094] Example 22 A concentrated sugar syrup was prepared at 60°C according to Example 12. An additional amount of sugar was sieved to obtain the 500-600 μm fraction, and the other fractions were discarded. 600 g of sieved sugar (500-600 μm fraction) was gradually added to the crystallizer over a period of 1 minute under constant mixing. Subsequently, 4 g of silica (Flo-gard™ T-800) was gradually added over a period of 30 seconds, again under constant mixing. This amount represents approximately 0.33% by weight of pure silica relative to the total amount of sugar in the process (i.e., in the syrup + sieved sugar).
[0095] Solid / liquid separation was performed according to Example 8 with a centrifugation time of 40 seconds. Drying of the silica- and sugar-coated sugar was performed by means of a fluidized bed dryer according to the procedure provided in Example 8A. The average concentration of pure silica relative to the average concentration of sugar within the coated sugar particles was approximately 0.08%.
[0096] Example 23 A concentrated sugar syrup was prepared at 60°C according to Example 12. An additional amount of sugar was sieved to obtain the 500-600 μm fraction, and the other fractions were discarded. 600 g of sieved sugar (500-600 μm fraction) was gradually added to the crystallizer over a period of 1 minute under constant mixing. Subsequently, 4 g of silica (Flo-gard™ T-800) was gradually added over a period of 30 seconds, again under constant mixing. This amount represents approximately 0.33% by weight of pure silica relative to the total amount of sugar in the process (i.e., in the syrup + sieved sugar).
[0097] Solid / liquid separation was performed according to Example 8 with a centrifugation time of 25 seconds. Drying of the silica- and sugar-coated sugar was performed by means of a fluidized bed dryer according to the procedure provided in Example 8A. The average concentration of pure silica relative to the average concentration of sugar within the coated sugar particles was approximately 0.11%.
[0098] Example 24 Example 19 was repeated using sorbitol instead of sugar. The average concentration of pure silica relative to the average concentration of sugar in the coated sugar particles was approximately 0.10%.
[0099] Example 25 Example 16 was repeated using sorbitol instead of sugar. The average concentration of pure silica relative to the average concentration of sugar in the coated sugar particles was approximately 0.12%.
[0100] Example 26: Etching of Silica- and Sweetener-Coated Sweetener Particles To characterize the outer layer of the coated sweetener particles, the coated sweetener particles were subjected to an etching process. Those skilled in the art will understand that the etching process can be designed to remove a portion of the coating without dissolving (or very slightly dissolving) any of the sweetener kernels. Alternatively, the etching process can be designed to remove substantially all of the coating while dissolving only a portion or small portion of the sweetener kernels.
[0101] Each fraction from the etching process can be treated and analyzed separately to determine its respective concentration of silica.
[0102] For sugar (typically sucrose), for example, a mixture of ethanol and water (4:1 w:w) is used as the etching solvent. Typically, a sugar sample is sieved using ASTM Sieves No. 30 and 35 to obtain a 500-595 μm fraction. 10 g of this fraction of sugar is mixed with 50 ml of an EtOH:water mixture using an overhead stirrer at 400 rpm for 12 minutes. The resulting slurry is filtered, and the cake (containing the "etched" sugar particles) is oven-dried overnight at 65°C. An ash test is performed on the etched sugar to assess the silica concentration. This concentration can be compared to the silica concentration in the initial sample of coated sugar (which can be quantified by the same ash test) and / or the silica concentration in the dried filtrate (which can also be quantified by the same ash test). The silica concentration in the dried filtrate represents the silica concentration in the etched fraction.
[0103] It will be understood by those skilled in the art that a variety of analytical techniques can be used to characterize the outer layer or coating of the silica-and-sweetener coated sweetener particles and compare its properties to the properties of the material underlying the coating.
[0104] Example 27 A dispersion (slurry) containing 50% amorphous silica and 50% sucrose was prepared according to Example 9 by slowly adding 100 grams of silica to a sucrose syrup containing 100 grams of sucrose and 500 grams of water. The silica-containing syrup was then transferred to a heated double-jacketed vessel of a vacuum dryer and heated and maintained under vacuum according to Example 9A to produce a silica-sweetener concentrate as a fine dry powder.
[0105] Example 28 A dispersion (slurry) containing 70% amorphous silica and 30% sucrose was prepared according to Example 9 by slowly adding 100 grams of silica to a sucrose syrup containing 42.8 grams of sucrose and 500 grams of water. The silica-containing syrup was then transferred to a heated double-jacketed vessel of a vacuum dryer and heated and maintained under vacuum according to Example 9A to produce a silica-sweetener concentrate as a fine dry powder.
[0106] Example 29 A dispersion (slurry) containing 10% amorphous silica and 90% sucrose was prepared according to Example 9 by slowly adding 100 grams of silica to a sucrose syrup containing 900 grams of sucrose and 500 grams of water. The silica-containing syrup was then transferred to a heated double-jacketed vessel of a vacuum dryer and heated and maintained under vacuum according to Example 9A to produce a silica-sweetener concentrate as a fine dry powder.
[0107] Example 30 A dispersion (slurry) containing 30% amorphous silica and 70% sucrose was prepared according to Example 9 by slowly adding 100 grams of silica to a sucrose syrup containing 233.3 grams of sucrose and 500 grams of water. The silica-containing syrup was then transferred to a heated double-jacketed vessel of a vacuum dryer and heated and maintained under vacuum according to Example 9A to produce a silica-sweetener concentrate as a fine dry powder.
[0108] Example 31 A dispersion containing 1% amorphous silica and 99% sucrose was prepared according to Example 9, and 650 grams of concentrated sweetener syrup containing sucrose was prepared before adding the silica. 6.5 grams of silica was then dispersed in the concentrated sweetener syrup. The syrup was transferred to a heated double-jacketed vessel in a vacuum dryer and heated and maintained under vacuum according to Example 9A to produce a silica-sweetener concentrate as a fine dry powder.
[0109] Example 32 A dispersion containing 1.5% amorphous silica and 98.5% sucrose was prepared according to Example 9, and a concentrated sweetener syrup containing 650 grams of sucrose was prepared before adding the silica. 9.75 grams of silica was then dispersed in the concentrated sweetener syrup. The syrup was transferred to a heated double-jacketed vessel in a vacuum dryer and heated and maintained under vacuum according to Example 9A to produce a silica-sweetener concentrate as a fine dry powder.
[0110] Example 33 A dispersion (slurry) containing 40% amorphous silica and 60% sucrose was prepared according to Example 9 by slowly adding 100 grams of silica to a sucrose syrup containing 150 grams of sucrose and 500 grams of water. The silica-containing syrup was then transferred to a heated double-jacketed vessel of a vacuum dryer and heated and maintained under vacuum according to Example 9A to produce a silica-sweetener concentrate as a fine dry powder.
[0111] Example 34 A dispersion (slurry) containing 20% amorphous silica and 80% sucrose was prepared according to Example 9 by slowly adding 100 grams of silica to a sucrose syrup containing 400 grams of sucrose and 500 grams of water. The silica-containing syrup was then transferred to a heated double-jacketed vessel of a vacuum dryer and heated and maintained under vacuum according to Example 9A to produce a silica-sweetener concentrate as a fine dry powder.
[0112] Example 35 A dispersion (slurry) containing 60% amorphous silica and 40% sucrose was prepared according to Example 9 by slowly adding 100 grams of silica to a sucrose syrup containing 66.6 grams of sucrose and 500 grams of water. The silica-containing syrup was then transferred to a heated double-jacketed vessel of a vacuum dryer and heated and maintained under vacuum according to Example 9A to produce a silica-sweetener concentrate as a fine dry powder.
[0113] Examples 36 to 44 The formulations of Examples 27-35 were prepared, but using fructose instead of sucrose.
[0114] Example 45 A silica-sweetener concentrate was produced by processing the formulation of Example 27 according to Example 9, followed by heating under vacuum according to Example 9A to produce the silica-sweetener concentrate as a fine, dry powder. The powder was subjected to size reduction according to Example 9B. The milled silica-sweetener concentrate powder was then mixed with regular sugar according to Example 10, i.e., 0.16 grams of powder was mixed with 79.84 grams of sucrose to yield 80 grams of a final sweetener formulation containing an average silica concentration of 0.1%.
[0115] Example 46 A silica-sweetener concentrate was produced by processing the formulation of Example 33 according to Example 9, followed by heating under vacuum according to Example 9A to produce the silica-sweetener concentrate as a fine, dry powder. The powder was subjected to size reduction according to Example 9B. The milled silica-sweetener concentrate powder was then mixed with regular sugar according to Example 10, i.e., 0.2 grams of powder was mixed with 79.8 grams of sucrose to yield 80 grams of a final sweetener formulation containing an average silica concentration of 0.1%.
[0116] Example 47 A silica-sweetener concentrate was produced by processing the formulation of Example 29 according to Example 9, followed by heating under vacuum according to Example 9A to produce the silica-sweetener concentrate as a fine, dry powder. The powder was subjected to size reduction according to Example 9B. The milled silica-sweetener concentrate powder was then mixed with regular sugar according to Example 10, i.e., 0.8 grams of powder was mixed with 79.2 grams of sucrose to yield 80 grams of a final sweetener formulation containing an average silica concentration of 0.1%.
[0117] Example 48 A silica-sweetener concentrate was produced by processing the formulation of Example 29 according to Example 9, followed by evaporation under vacuum according to Example 9A to produce the silica-sweetener concentrate as a fine dry powder. The powder was subjected to size reduction according to Example 9B. The silica-sweetener concentrate powder was then mixed with regular sugar according to Example 10, i.e., 5 grams of powder was mixed with 95 grams of sucrose to obtain 100 grams of a final sweetener formulation containing an average silica concentration of 0.5%.
[0118] Example 49 A silica-sweetener concentrate was produced by processing the formulation of Example 27 according to Example 9, followed by heating under vacuum according to Example 9A to produce the silica-sweetener concentrate as a fine, dry powder. The powder was subjected to size reduction according to Example 9B. The milled silica-sweetener concentrate powder was then mixed with regular sugar according to Example 10, i.e., 1.6 grams of powder was mixed with 78.4 grams of sucrose to yield 80 grams of a final sweetener formulation containing an average silica concentration of 1%.
[0119] Example 50 A silica-sweetener concentrate was produced by processing the formulation of Example 27 according to Example 9, followed by heating under vacuum according to Example 9A to produce the silica-sweetener concentrate as a fine, dry powder. The powder was subjected to size reduction according to Example 9B. The milled silica-sweetener concentrate powder was then mixed with regular sugar according to Example 10, i.e., 0.08 grams of powder was mixed with 79.92 grams of sucrose to yield 80 grams of a final sweetener formulation containing an average silica concentration of 0.05%.
[0120] Example 51 A silica-sweetener concentrate was produced by processing the formulation of Example 29 according to Example 9, followed by heating under vacuum according to Example 9A to produce the silica-sweetener concentrate as a fine, dry powder. The powder was subjected to size reduction according to Example 9B. The milled silica-sweetener concentrate powder was then mixed with regular sugar according to Example 10, i.e., 1.6 grams of powder was mixed with 78.4 grams of sucrose to yield 80 grams of a final sweetener formulation containing an average silica concentration of 0.2%.
[0121] Example 52 A silica-sweetener concentrate was produced by processing the formulation of Example 27 according to Example 9, followed by heating under vacuum according to Example 9A to produce the silica-sweetener concentrate as a fine, dry powder. The powder was subjected to size reduction according to Example 9B. The milled silica-sweetener concentrate powder was then mixed with regular sugar according to Example 10, i.e., 0.32 grams of powder was mixed with 79.68 grams of sucrose to yield 80 grams of a final sweetener formulation containing an average silica concentration of 0.2%.
[0122] Example 53 A silica-sweetener concentrate was produced by processing the formulation of Example 30 according to Example 9, followed by heating under vacuum according to Example 9A to produce the silica-sweetener concentrate as a fine, dry powder. The powder was subjected to size reduction according to Example 9B. The milled silica-sweetener concentrate powder was then mixed with regular sugar according to Example 10, i.e., 0.5 grams of powder was mixed with 99.5 grams of sucrose to yield 100 grams of a final sweetener formulation containing an average silica concentration of 0.15%.
[0123] Example 54 A silica-sweetener concentrate was produced by processing the formulation of Example 29 according to Example 9, followed by heating under vacuum according to Example 9A to produce the silica-sweetener concentrate as a fine dry powder. The powder was subjected to size reduction according to Example 9B. The milled silica-sweetener concentrate powder was then mixed with regular sugar according to Example 3, i.e., 1.6 grams of powder was mixed with 78.4 grams of sucrose to yield 80 grams of a final sweetener formulation containing an average silica concentration of 0.2%.
[0124] Example 55 A silica-sweetener concentrate was produced by processing the formulation of Example 29 according to Example 9, followed by heating under vacuum according to Example 9A to produce the silica-sweetener concentrate as a fine, dry powder. The powder was subjected to size reduction according to Example 9B. The milled silica-sweetener concentrate powder was then mixed with regular sugar according to Example 10, i.e., 0.5 grams of powder was mixed with 99.5 grams of sucrose to yield 100 grams of a final sweetener formulation containing an average silica concentration of 0.05%.
[0125] Example 56 A silica-sweetener concentrate was produced by processing the formulation of Example 32 according to Example 9, followed by heating under vacuum according to Example 9A to produce the silica-sweetener concentrate as a fine, dry powder. The powder was subjected to size reduction according to Example 9B. The milled silica-sweetener concentrate powder was then blended with regular sugar according to Example 10, i.e., 16 grams of powder was blended with 84 grams of sucrose to yield 100 grams of a final sweetener formulation containing an average silica concentration of 0.24%.
[0126] Example 57 A silica-sweetener concentrate was produced by processing the formulation of Example 33 according to Example 9, followed by heating under vacuum according to Example 9A to produce the silica-sweetener concentrate as a fine, dry powder. The powder was subjected to size reduction according to Example 9B. The milled silica-sweetener concentrate powder was then mixed with regular sugar according to Example 10, i.e., 2.5 grams of powder was mixed with 97.5 grams of sucrose to yield 100 grams of a final sweetener formulation containing an average silica concentration of 1%.
[0127] Example 58 A silica-sweetener concentrate was produced by processing the formulation of Example 30 according to Example 9, followed by heating under vacuum according to Example 9A to produce the silica-sweetener concentrate as a fine, dry powder. The powder was subjected to size reduction according to Example 9B. The milled silica-sweetener concentrate powder was then mixed with regular sugar according to Example 10, i.e., 0.166 grams of powder was mixed with 99.833 grams of sucrose to yield 100 grams of a final sweetener formulation containing an average silica concentration of 0.05%.
[0128] Example 59 A silica-sweetener concentrate was produced by processing the formulation of Example 30 according to Example 9, followed by heating under vacuum according to Example 9A to produce the silica-sweetener concentrate as a fine, dry powder. The powder was subjected to size reduction according to Example 9B. The milled silica-sweetener concentrate powder was then mixed with regular sugar according to Example 10, i.e., 0.5 grams of powder was mixed with 99.5 grams of sucrose to yield 100 grams of a final sweetener formulation containing an average silica concentration of 0.15%.
[0129] Example 60 A silica-sweetener concentrate was produced by processing the formulation of Example 34 according to Example 9, followed by heating under vacuum according to Example 9A to produce the silica-sweetener concentrate as a fine, dry powder. The powder was subjected to size reduction according to Example 9B. The milled silica-sweetener concentrate powder was then mixed with regular sugar according to Example 10, i.e., 0.5 grams of powder was mixed with 99.5 grams of sucrose to yield 100 grams of a final sweetener formulation containing an average silica concentration of 0.1%.
[0130] Example 61 A silica-sweetener concentrate was produced by processing the formulation of Example 35 according to Example 9, followed by heating under vacuum according to Example 9A to produce the silica-sweetener concentrate as a fine, dry powder. The powder was subjected to size reduction according to Example 9B. The milled silica-sweetener concentrate powder was then mixed with regular sugar according to Example 10, i.e., 0.6 grams of powder was mixed with 79.4 grams of sucrose to yield 80 grams of a final sweetener formulation containing an average silica concentration of 0.45%.
[0131] Example 62 A dispersion (slurry) containing 30% silica and 70% allulose was prepared according to Example 9, i.e., 51.5 grams of amorphous silica was gradually added to an allulose syrup containing 120 grams of allulose and 480 grams of water. The silica-containing syrup was then transferred to a heated double-jacketed vessel of a vacuum dryer and heated and maintained under vacuum according to Example 9A to produce a silica-sweetener concentrate as a fine dry powder.
[0132] Example 63 A silica-sweetener concentrate was produced by treating the formulation of Example 28 according to Example 9, followed by heating under vacuum according to Example 9A to produce the silica-sweetener concentrate as a fine dry powder. The powder was subjected to size reduction according to Example 9B. The silica-sweetener concentrate powder was then mixed with allulose according to Example 10, i.e., 0.32 grams of powder was mixed with 79.68 grams of allulose to yield 80 grams of a final sweetener formulation containing an average silica concentration of 0.28%.
[0133] Examples 64 to 72 The formulations of Examples 27-35 were prepared, but using maltitol instead of sucrose and 700 g of water.
[0134] Examples 73 to 81 The formulations of Examples 27-35 were prepared, but using sorbitol instead of sucrose and 700 g of water.
[0135] Example 82: Preparation of muffin samples Three muffin samples can be prepared: Type I is a "full sugar" control muffin, which can be similar in composition to a typical commercial muffin; Type II is a reduced sugar muffin of the present invention containing a silica-sweetener or silica-sweetener concentrate of the present invention; and Type III is a reduced sugar control muffin, which has the same composition as Type II of the reduced sugar muffin of the present invention, but lacks silica in the sweetener particles.
[0136] The batter for each type of muffin contains sugar, 14.2% sunflower oil, 21.8% wheat flour (containing about 40% starch), 24.5% eggs, 1.1% baking powder, 0.1% flavoring or seasoning, 0.1% salt, and about 16.4% water. The batter for the I-type muffins contains 21.8% sugar by weight.
[0137] Fructooligosaccharides are used as bulking agents to compensate for the reduced amount of sugars in Type II and Type III samples, typically Gofos™ (which typically contains 2% sugars) is used.
[0138] Type II muffins utilize sweetener blends from a variety of exemplary blends, many of which are described or exemplified above. Aside from the differences in blends, the preparation and baking processes for the inventive and control muffins are the same.
[0139] Example 82A Typically, Type II reduced sugar muffins of the present invention contain 39.1% less sugar than the Type I "full sugar" control muffin. In this exemplary case, Types II and III muffins contain approximately (100% - 39.1%) x 21.8% = 13.3% sugar by weight of the dough. The fructooligosaccharide (Gofos™) content of the muffin dough is approximately 8.5% by weight (21.8% - 13.38%).
[0140] Example 82B In many cases, Type II reduced sugar muffins of the present invention can contain reduced sugars in amounts other than the typical reduction of 39.1%. By way of (non-exhaustive) example, Type II muffins may contain 50% less sugar, 35% less sugar, 20% less sugar, or 10% less sugar. In the exemplary case of 20% less sugar, a Type II muffin would be formulated so that the dough contains approximately (100% - 20%) x 21.8% = 17.44% sugar by weight, and 4.36% Gofos™ (21.8% - 17.44%) by weight. In each case, strictly for comparative purposes, the Type II muffin contains at least 10% less sugar than the Type I "full sugar" control muffin.
[0141] Example 83: Butter Cookie Sample Preparation Three types of butter cookie samples can be prepared: Type I is a "full sugar" control butter cookie, which can have a composition similar to a typical commercially available butter cookie; Type II is a low-sugar butter cookie of the present invention containing a silica-sweetener or silica-sweetener concentrate of the present invention; and Type III is a low-sugar control butter cookie, which has the same composition as Type II of the low-sugar butter cookie of the present invention, but lacks silica in the sweetener particles.
[0142] The dough for each type of butter cookie contains sugar, 14.6% palm oil, 49.42% wheat flour (containing about 40% starch), cornstarch (4.2%), water (5.7%), eggs (3.6%), soy lecithin (0.19%), baking powder (0.3%), salt (0.2%), 1.2% invert sugar (containing 5% water), 1.5% heavy cream (containing 37% fat and 3.5% lactose), flavoring or flavoring (0.1%), and the remainder is water. The sugar content of Type I butter cookies is about 19.0%.
[0143] Inulin is used as a bulking agent to make up for the reduced amount of sugars in Type II and Type III samples. Orafti highly soluble inulin (containing 10% sugars) is typically utilized.
[0144] The Type II butter cookies utilize sweetener blends from a variety of exemplary formulations, many of which are described or exemplified above. Aside from the differences in formulation, the preparation and baking processes for the inventive and control butter cookies are the same.
[0145] Example 83A Typically, Type II reduced-sugar butter cookies of the present invention contain about 40% less sugar than Type I "full sugar" control butter cookies. In this illustrative example, Type II and Type III butter cookies have a dough containing about (100% - 40.45%) x 19.0% = 11.3% sugar by weight. The inulin content of the dough is about 7.7% by weight (19.0% - 11.3%). Essentially, as with the muffin sample provided above, Type II reduced-sugar butter cookies of the present invention may often contain reduced sugar in amounts other than the typical reduction of about 40%. By way of (non-exhaustive) example, Type II butter cookies may contain 50% less sugar, 40% less sugar, 35% less sugar, 20% less sugar, or 10% less sugar. Strictly for comparative purposes, Type II butter cookies contain at least 10% less sugar than Type I "full sugar" control butter cookies.
[0146] Example 84: Preparation of hazelnut spread samples Three types of hazelnut spread samples can be prepared. Type I is a "full sugar" control hazelnut spread, which can be similar in composition to typical commercial hazelnut spreads. Type II is the reduced-sugar hazelnut spread of the present invention, which contains the silica-sweetener or silica-sweetener concentrate of the present invention. Type III is the reduced-sugar control hazelnut spread, which has the same composition as the reduced-sugar hazelnut spread of Type II of the present invention, but lacks silica in the sweetener particles.
[0147] Each type of hazelnut spread contains sugar, hazelnut paste (13%), palm oil (23.7%), cocoa powder with 12% fat (7.4%), skimmed milk powder (6.6%), rapeseed lecithin (0.2%), and flavors or aromas (0.1%). The sugar content of Type I hazelnut spread is 49%.
[0148] Fructooligosaccharides are used as bulking agents to compensate for the reduced amount of sugar in Type II and Type III samples. Inulin is usually used. Type II hazelnut spread uses sweetener compounds from various exemplary compounds (many of which are described or exemplified above). Except for the difference in compounding, the preparation process of the hazelnut spread of the present invention and the control hazelnut spread is the same.
[0149] Example 84A Typically, Type II of the reduced sugar hazelnut spread of the present invention contains about 41% less sugar than Type I of the "full sugar" control hazelnut spread. In this exemplary case, Type II and Type III hazelnut spreads are formulated to contain about (100% - 30%) x 49% = 34.3% by weight of sugar. The inulin content of the hazelnut spreads is about 14.7% by weight (49% - 34.3%).
[0150] In many cases, as in the case of the hazelnut spread samples provided above, Type II reduced sugar hazelnut spread of the present invention may contain reduced sugar in amounts other than the usual 30% reduction.As a (non-exhaustive) example, Type II hazelnut spread may contain 50% less sugar, 35% less sugar, 20% less sugar, or 10% less sugar.Strictly for comparison purposes, Type II hazelnut spread contains at least 10% less sugar compared to Type I "full sugar" control hazelnut spread.
[0151] Example 85: Sensory evaluation Exemplary sweeteners or edible formulations (e.g., muffins, butter cookies, and hazelnut spreads) can be evaluated by trained sensory panelists using paired comparison tests. Paired comparison tests are two-product blind tests in which the panelist's task is to select / indicate the sweeter of the two products or samples (Sensory Evaluation Practices, 4 th(Eds., Stone, Bleibaum, Thomas, eds.). Results are analyzed using a binomial distribution table, which allows the sensory scientist to determine whether the perceived differences between samples are statistically significant. A comparative sweetness index can be calculated from the paired comparison test results collected from all panelists. For example, if, of 17 panelists, 10 selected the product of the present invention as sweeter, while the other 7 panelists selected the comparison or control product, the comparative sweetness index (CSI) would be calculated as follows: CSI=(10 / 17)×100=58.8=59(rounded off)
[0152] Example 85A Another sensory method used to evaluate samples is the Difference Magnitude Estimation (DME), where each panelist tastes two samples, chooses the sweetest, and selects the difference in sweetness from the following list: There is no difference at all Very small difference A small difference Moderate difference Big difference A huge difference
[0153] Each option is given a numerical value (0-5) and the panel's average is calculated (the value is considered positive if the first (inventive, silica-containing) sample is indicated as sweeter, and vice versa). Generally, differences of up to ±1.0 (i.e., within an absolute value of 1), and in some cases, differences of up to ±0.8 or up to ±0.5, are considered insignificant (i.e., the sweetness of the samples is substantially the same). Insignificant differences are considered to be good results for the comparison of the inventive formulation with the control formulation.
[0154] Examples 86-87 Muffin samples were prepared using the various formulations exemplified above according to Examples 82 and 82A. The paired comparison test results of the paired comparison tests conducted and evaluated according to Examples 85 and 85A are listed in Table 1 below.
[0155] Examples 88 to 91 Butter cookie samples were prepared using the various formulations exemplified above according to Examples 83 and 83A. The paired comparison test results of the paired comparison tests conducted and evaluated according to Examples 85 and 85A are listed in Table 1 below.
[0156] Examples 92-93 Using various formulations as exemplified above, hazelnut spread samples are prepared according to Example 84 and 84A.The paired comparison test results of the paired comparison test carried out and evaluated according to Example 85 and 85A are listed in the following table 1. [Table 3]
[0157] Example 94—Comparative Dissolution Rates Dissolution rates were tested comparing sucrose formulations containing low concentrations of amorphous silica with a crystalline sucrose control formulation. The temperature of the stirring vessel was maintained at 37°C (to simulate body temperature). For the control sample, crystalline sugar (sucrose) was milled to approximate the particle size of the silica-sweetener concentrate. 5.0 g of milled sugar was added to a stirring vessel containing 500 ml of water, and the concentration of dissolved sugar was monitored over time. Three samples were evaluated against the control: Sample A, in which the sucrose particles contained 0.1% amorphous silica; Sample B, in which the sucrose particles contained 0.25% amorphous silica; and Sample C, in which the sucrose particles contained 1% amorphous silica.
[0158] Each sample was then introduced into a stirred vessel containing 500 ml of water maintained at 37°C (to simulate body temperature). In each of the four tests, a total of 5.0 g of sugar was introduced at t=0. For sweetener particles containing amorphous silica, a silica-sweetener concentrate sample was used, which was the concentrate of Example 27 containing 50% amorphous silica and 50% sucrose. 10.0 g of concentrate containing the same amount of sucrose (5.0 g) as the control sample was added to a stirred vessel containing 500 g of water. Mixing and heating were performed in the same manner as for the control sample. The results are plotted in Figure 6A.
[0159] This procedure, in which the total sugar concentration is 1% by weight and the vessel is well stirred and maintained at 37°C, is referred to as the "standard rate evaluation procedure."
[0160] Example 95—Comparative Dissolution Rates Dissolution rates were tested comparing sucrose formulations containing high concentrations of amorphous silica with a crystalline sucrose control formulation. The temperature of the stirring vessel was maintained at 37°C. For the control sample, crystalline sugar (sucrose) was milled to approximate the particle size of the silica-sweetener concentrate. 5.0 g of the milled sugar was added to a stirring vessel containing 500 ml of water, and the concentration of dissolved sugar was monitored over time. For the silica-sweetener concentrate sample of the present invention, the concentrate of Example 27, whose particles contain 50% amorphous silica and 50% sucrose, was used. 10.0 grams of the concentrate containing the same amount of sucrose (5.0 g) as the control sample, was added to a stirring vessel containing 500 ml of water. Mixing and heating were performed in the same manner as for the control sample. The results are plotted in Figure 6B.
[0161] Examples 96 to 98 Two silica-and-sweetener concentrates, 25:75 and 15:85 silica:sucrose by weight, were subjected to X-ray diffraction (XRD) using an X-ray diffractometer (D8 Advance Series II, Bruker). As a control, table sugar was subjected to the same procedure. The respective diffraction patterns (intensity vs. 2θ) are plotted in Figure 7.
[0162] From the XRD plot of the concentrate, it is clear that the diffraction pattern of the concentrate exhibits crystalline characteristics and is qualitatively similar to that of a crystalline sucrose sample.
[0163] It will be understood that quantification of the degree of crystallinity, or the relative amount of amorphous sweetener to crystalline sweetener (e.g., as used herein in this specification and the claims section below), can be determined by a variety of analytical procedures known to those skilled in the art, including, but not limited to, the following: X-ray powder diffraction (XRPD) ●Isothermal microcalorimeter (IMC) Solution calorimetry Dynamic Vapor Sorption (DVS) ● Conventional differential scanning calorimetry (DSC), temperature modulated DSC (MTDSC), high-speed DSC (high DSC) Raman spectroscopy ●Near infrared spectroscopy (NIRS) ●Solid-state nuclear magnetic resonance method (SS-NMR) Inverse gas chromatography (IGC) ●Density (specific gravity) measurement.
[0164] Example 99: Exemplary Starch Content Calculations The cookies are made from fat (palm oil, 17%), white wheat flour (61%), sucrose (11%), the silica-sweetener concentrate of Example 8 (1%), and fructan (inulin, 10%). The only starch-containing ingredient is white wheat flour, which contains approximately 68% starch. Therefore, the starch content of the cookies is 68% of 61%, or approximately 41.5%.
[0165] Example 100: Exemplary Fat Content Calculations The hazelnut spread is made from fat (palm oil, 24%), sucrose (28%), silica-sweetener concentrate of Example 11 (2%), pure hazelnut paste (13%, having a fat content of 61%), non-fat milk powder (6%), cocoa powder (7%, having a fat content of 12%), and fructan (inulin, 20%). The total fat content of the hazelnut spread is 24% + (13% of 61%) + (7% of 12%) or approximately 32.8%.
[0166] Additional Embodiments Additional embodiments 1-152 are provided below.
[0167] Embodiment 1. A formulation comprising: a population of first sweetener particles containing a plurality of amorphous silica particles within the population of first sweetener particles; Each individual sweetener particle of said sweetener particles comprises: (a) a caloric sweetener; (b) at least one amorphous silica particle disposed within each individual sweetener particle; the first population has an average particle size (Dv50-P) in the range of 20 to 1000 micrometers (μm); The average particle size (Dv50-S) of the plurality of amorphous silica particles is within the range of 0.8 to 20 micrometers (μm), an average ratio of the number of said plurality of amorphous silica particles to the number of said sweetener particles of at least 2.5:1; the population of first sweetener particles is less sweet than a control sweetener identical to the population of first sweetener particles but lacking the plurality of amorphous silica particles; The formulation, wherein when the first population is diluted with sucrose to produce a standard formulation containing 0.1% amorphous silica, the standard formulation exhibits improved sweetness relative to a corresponding control sucrose formulation identical to the standard formulation but lacking the plurality of amorphous silica particles.
[0168] Embodiment 2. The formulation of embodiment 1, wherein each individual sweetener particle has a sweetener core devoid of amorphous silica particles, the sweetener core having a diameter of at least 7 micrometers (μm), and the sweetener core is disposed at least 5 micrometers (μm) from the surface of each individual sweetener particle.
[0169] Embodiment 3. The formulation of embodiment 2, wherein the diameter of the sweetener core is at least 10 μm.
[0170] Embodiment 4. The formulation of embodiment 2, wherein the diameter of the sweetener core is at least 15 μm.
[0171] Embodiment 5. The formulation of embodiment 2, wherein the diameter of the sweetener core is at least 25 μm.
[0172] Embodiment 6. The formulation of embodiment 2, wherein the diameter of the sweetener core is at least 40 μm.
[0173] Embodiment 7. The formulation of embodiment 2, wherein the diameter of the sweetener core is at least 60 μm.
[0174] Embodiment 8. The formulation of any one of embodiments 1 to 7, wherein the average ratio of the number of amorphous silica particles to the number of sweetener particles is at least 3.5:1.
[0175] Embodiment 9. The formulation of any one of embodiments 1 to 7, wherein the average ratio of the number of amorphous silica particles to the number of sweetener particles is at least 5:1.
[0176] Embodiment 10. A formulation according to any one of embodiments 1 to 7, wherein the average ratio of the number of amorphous silica particles to the number of sweetener particles is at least 7:1.
[0177] Embodiment 11. A formulation according to any one of embodiments 1 to 7, wherein the average ratio of the number of amorphous silica particles to the number of sweetener particles is at least 10:1.
[0178] Embodiment 12. A formulation according to any one of embodiments 1 to 7, wherein the average ratio of the number of amorphous silica particles to the number of sweetener particles is at least 15:1.
[0179] Embodiment 13. A formulation according to any one of embodiments 1 to 12, wherein the average ratio of the number of amorphous silica particles to the number of sweetener particles is at most 250:1.
[0180] Embodiment 14. The formulation of embodiment 13, wherein the average ratio of the number of amorphous silica particles to the number of sweetener particles is at most 150:1.
[0181] Embodiment 15. The formulation of embodiment 13, wherein the average ratio of the number of amorphous silica particles to the number of sweetener particles is at most 100:1.
[0182] Embodiment 16. A formulation according to any one of the preceding embodiments, wherein Dv50-P is at least 25 μm.
[0183] Embodiment 17. A formulation according to embodiment 16, wherein Dv50-P is at least 30 μm.
[0184] Embodiment 18. A formulation according to embodiment 16, wherein the Dv50-P is at least 35 μm.
[0185] Embodiment 19. A formulation according to embodiment 16, wherein Dv50-P is at least 40 μm.
[0186] Embodiment 20. A formulation according to embodiment 16, wherein Dv50-P is at least 50 μm.
[0187] Embodiment 21. A formulation according to embodiment 16, wherein the Dv50-P is at least 65 μm.
[0188] Embodiment 22. A formulation according to embodiment 16, wherein Dv50-P is at least 80 μm.
[0189] Embodiment 23. A formulation according to embodiment 16, wherein Dv50-P is at least 100 μm.
[0190] Embodiment 24. A formulation according to embodiment 16, wherein the Dv50-P is at least 125 μm.
[0191] Embodiment 25. A formulation according to embodiment 16, wherein Dv50-P is at least 150 μm.
[0192] Embodiment 26. A formulation according to any one of the preceding embodiments, wherein Dv50-S is at least 1 μm.
[0193] Embodiment 27. A formulation according to embodiment 26, wherein the Dv50-S is at least 1.5 μm.
[0194] Embodiment 28. A formulation according to embodiment 26, wherein Dv50-S is at least 2 μm.
[0195] Embodiment 29. A formulation according to embodiment 26, wherein Dv50-S is at least 2.5 μm.
[0196] Embodiment 30. A formulation according to any one of the preceding embodiments, wherein Dv50-S is up to 15 μm.
[0197] Embodiment 31. A formulation according to embodiment 26, wherein Dv50-S is at most 10 μm.
[0198] Embodiment 32. The formulation of any one of the preceding embodiments, wherein a first weight ratio of the plurality of amorphous silica particles to the caloric sweetener is in the range of 0.07:1 to 10:1.
[0199] Embodiment 33. The formulation of embodiment 32, wherein the first weight ratio is at least 0.10:1.
[0200] Embodiment 34. The formulation of embodiment 32, wherein the first weight ratio is at least 0.12:1.
[0201] Embodiment 35. The formulation of embodiment 32, wherein the first weight ratio is at least 0.15:1.
[0202] Embodiment 36. The formulation of embodiment 32, wherein the first weight ratio is at least 0.20:1.
[0203] Embodiment 37. The formulation of embodiment 32, wherein the first weight ratio is at least 0.25:1.
[0204] Embodiment 38. The formulation of embodiment 32, wherein the first weight ratio is at least 0.30:1.
[0205] Embodiment 39. The formulation of embodiment 32, wherein the first weight ratio is at least 0.35:1.
[0206] Embodiment 40. The formulation of embodiment 32, wherein the first weight ratio is at least 0.40:1.
[0207] Embodiment 41. The formulation of embodiment 32, wherein the first weight ratio is at least 0.45:1.
[0208] Embodiment 42. The formulation of embodiment 32, wherein the first weight ratio is at least 0.5:1.
[0209] Embodiment 43. The formulation of embodiment 32, wherein the first weight ratio is at least 0.6:1.
[0210] Embodiment 44. The formulation of embodiment 32, wherein the first weight ratio is at least 0.7:1.
[0211] Embodiment 45. The formulation of embodiment 32, wherein the first weight ratio is at least 0.8:1.
[0212] Embodiment 46. The formulation of embodiment 32, wherein the first weight ratio is at least 0.9:1.
[0213] Embodiment 47. The formulation of embodiment 32, wherein the first weight ratio is at least 1:1.
[0214] Embodiment 48. The formulation of embodiment 32, wherein the first weight ratio is at least 1.2:1.
[0215] Embodiment 49. The formulation of embodiment 32, wherein the first weight ratio is at least 1.5:1.
[0216] Embodiment 50. The formulation of embodiment 32, wherein the first weight ratio is at least 2:1.
[0217] Embodiment 51. The formulation of any one of the preceding embodiments, wherein within the first population, at least 50% by number of molecular units of the caloric sweetener are attached only to other molecular units of the caloric sweetener.
[0218] Embodiment 52. The formulation of embodiment 51, wherein at least 60% by number of molecular units of the caloric sweetener are attached only to other molecular units of the caloric sweetener.
[0219] Embodiment 53. A formulation according to embodiment 51, wherein at least 75% by number of molecular units of the caloric sweetener are attached only to other molecular units of the caloric sweetener.
[0220] Embodiment 54. The formulation of any one of the preceding embodiments, wherein up to 50% of the caloric sweetener disposed in the individual sweetener particles is directly bonded to any of the at least one amorphous silica particle.
[0221] Embodiment 55. The formulation of embodiment 54, wherein up to 40% of the caloric sweetener disposed in the individual sweetener particles is directly bound to the at least one amorphous silica particle.
[0222] Embodiment 56. The formulation of embodiment 54, wherein up to 30% of the caloric sweetener disposed in the individual sweetener particles is directly bound to the at least one amorphous silica particle.
[0223] Embodiment 57. The formulation of embodiment 54, wherein up to 20% of the caloric sweetener disposed in the individual sweetener particles is directly bound to the at least one amorphous silica particle.
[0224] Embodiment 58. The formulation of embodiment 54, wherein up to 10% of the caloric sweetener disposed in the individual sweetener particles is directly bound to the at least one amorphous silica particle.
[0225] Embodiment 59. The formulation of any one of the preceding embodiments, wherein up to 50% of the caloric sweetener disposed within each of the individual sweetener particles, on an average weight basis including all of the individual sweetener particles, is directly bonded to one of the at least one amorphous silica particle within the individual sweetener particle.
[0226] Embodiment 60. The formulation of embodiment 59, wherein up to 40% of the caloric sweetener disposed within each of the individual sweetener particles is directly bonded to one of the at least one amorphous silica particles within the individual sweetener particle.
[0227] Embodiment 61. The formulation of embodiment 59, wherein up to 30% of the caloric sweetener disposed within each individual sweetener particle is directly bonded to one of the at least one amorphous silica particle within the individual sweetener particle.
[0228] Embodiment 62. The formulation of embodiment 59, wherein up to 20% of the caloric sweetener disposed within each individual sweetener particle is directly bonded to one of the at least one amorphous silica particle within the individual sweetener particle.
[0229] Embodiment 63. The formulation of any one of the preceding embodiments, wherein the caloric sweetener comprises a sweetener carbohydrate selected from at least one of the group consisting of sucrose, glucose, fructose, maltose, lactose, mannose, allulose, tagatose, xylose, galactose, arabinose, and galactofructose.
[0230] Embodiment 64. A formulation according to embodiment 63, wherein the sweetener carbohydrate comprises sucrose.
[0231] Embodiment 65. The formulation of embodiment 63, wherein the sweetener carbohydrate comprises glucose.
[0232] Embodiment 66. A formulation according to embodiment 63, wherein the sweetener carbohydrate comprises fructose.
[0233] Embodiment 67. A formulation according to embodiment 63, wherein the sweetener carbohydrate comprises predominantly sucrose.
[0234] Embodiment 68. The formulation of embodiment 63, wherein the sweetener carbohydrate comprises primarily glucose.
[0235] Embodiment 69. A formulation according to embodiment 63, wherein the sweetener carbohydrate comprises predominantly fructose.
[0236] Embodiment 70. The formulation of any one of the preceding embodiments, wherein the caloric sweetener comprises a sweetener polyol selected from at least one of the group consisting of xylitol, maltitol, erythritol, sorbitol, threitol, arabitol, hydrogenated starch hydrolysates (HSH), isomalt, lactitol, mannitol, and galactitol (dulcitol).
[0237] Embodiment 71. A formulation according to any one of the preceding embodiments, wherein the sweetener formulation is in the form of a particulate solid.
[0238] Embodiment 72. The formulation of embodiment 71, wherein the particulate solid is a powder.
[0239] Embodiment 73. The formulation of embodiment 72, wherein the powder is a free-flowing powder.
[0240] Embodiment 74. The formulation of any one of the preceding embodiments, wherein the conventional sweetener is a standard conventional sweetener.
[0241] Embodiment 75. The formulation of any one of the preceding embodiments, wherein the regular sugar is a standard regular sugar.
[0242] Embodiment 76. The formulation of embodiment 75, wherein the standard normal sugar comprises sucrose.
[0243] Embodiment 77. The formulation of embodiment 75, wherein the normative regular sugar contains at least 65% sucrose by weight.
[0244] Embodiment 78. The formulation of embodiment 75, wherein the normative regular sugar contains at least 85% sucrose by weight.
[0245] Embodiment 79. The formulation of embodiment 75, wherein the normative regular sugar contains at least 95% sucrose by weight.
[0246] Embodiment 79A. A formulation described in any one of the preceding embodiments, wherein the difference in comparative sweetness index between the standard formulation and the corresponding control sucrose formulation that is identical to the standard formulation but lacks the plurality of amorphous silica particles is at least 3.
[0247] Embodiment 79B. The combination of embodiment 79A, wherein the difference is at least 5.
[0248] Embodiment 79C. The combination of embodiment 79A, wherein the difference is at least 7.
[0249] Embodiment 79D. The combination of embodiment 79A, wherein the difference is at least 10.
[0250] Embodiment 79E. The combination of embodiment 79A, wherein the difference is at least 15.
[0251] Embodiment 80. A formulation comprising: A first population of sweetener particles, wherein each individual sweetener particle of said sweetener particles comprises: (a) sweetener particles containing a caloric sweetener; (b) a plurality of amorphous silica particles disposed within each individual sweetener particle; the population of first sweetener particles exhibits a slower dissolution rate relative to a control sweetener identical to the population of first sweetener particles but lacking the plurality of amorphous silica particles; The formulation, wherein when the first population is diluted with the caloric sweetener to produce a standard formulation containing 0.1% amorphous silica, the standard formulation exhibits improved sweetness relative to a corresponding control sweetener formulation that is identical to the standard formulation but lacks the plurality of amorphous silica particles.
[0252] Embodiment 80A. A formulation comprising: A first population of sweetener particles, wherein each individual sweetener particle of said sweetener particles comprises: (a) sweetener particles containing a caloric sweetener; (b) a plurality of amorphous silica particles disposed within each individual sweetener particle; the population of first sweetener particles is the same as the population of second sweetener particles, but (i) devoid of said plurality of amorphous silica particles; (ii) exhibit a slower dissolution rate relative to a fully crystalline control sweetener; The formulation, wherein when the first population is diluted with the caloric sweetener to produce a standard formulation containing 0.1% amorphous silica, the standard formulation exhibits improved sweetness relative to a corresponding control sweetener formulation that is identical to the standard formulation but lacks the plurality of amorphous silica particles.
[0253] Embodiment 80B. A formulation comprising: A first population of sweetener particles, wherein each individual sweetener particle of said sweetener particles comprises: (a) sweetener particles containing a caloric sweetener; (b) a plurality of amorphous silica particles disposed within each individual sweetener particle; the population of first sweetener particles is the same as the population of second sweetener particles, but (i) devoid of said plurality of amorphous silica particles; (ii) exhibit a slower dissolution rate relative to a control sweetener that is completely amorphous; The formulation, wherein when the first population is diluted with the caloric sweetener to produce a standard formulation containing 0.1% amorphous silica, the standard formulation exhibits improved sweetness relative to a corresponding control sweetener formulation that is identical to the standard formulation but lacks the plurality of amorphous silica particles.
[0254] Embodiment 81. The formulation of any one of embodiments 1 to 80B, wherein the dissolution rate of the first population of sweetener particles is at least 5% slower than the dissolution rate of the control sweetener.
[0255] Embodiment 82. The formulation of embodiment 81, wherein the dissolution rate of the first population of sweetener particles is at least 7% slower.
[0256] Embodiment 83. The formulation of embodiment 81, wherein the dissolution rate of the first population of sweetener particles is at least 10% slower.
[0257] Embodiment 84. The formulation of embodiment 81, wherein the dissolution rate of the first population of sweetener particles is at least 12% slower.
[0258] Embodiment 85. The formulation of embodiment 81, wherein the dissolution rate of the first population of sweetener particles is at least 15% slower.
[0259] Embodiment 86. The formulation of embodiment 81, wherein the dissolution rate of the first population of sweetener particles is at least 20% slower.
[0260] Embodiment 87. The formulation of any one of embodiments 80-86, further comprising any one of the features or any combination of features of embodiments 1-79E.
[0261] Embodiment 100. A formulation comprising: A first population of sweetener particles, wherein each individual sweetener particle of said sweetener particles comprises: (a) a caloric sweetener; (b) at least one amorphous silica particle disposed within each sweetener particle; the first population has an average particle size (Dv50) in the range of 20 to 1000 micrometers (μm); The average particle size (Dv50) of the plurality of amorphous silica particles is within the range of 0.8 to 20 micrometers (μm), in at least a fraction of the sweetener particles of the first population of sweetener particles, up to 50% of the caloric sweetener is directly bound to the at least one amorphous silica particle; the population of first sweetener particles is less sweet than a control sweetener identical to the population of first sweetener particles but lacking the plurality of amorphous silica particles; The formulation, wherein when the first population is diluted with the caloric sweetener to produce a standard formulation containing 0.1% amorphous silica, the standard formulation exhibits improved sweetness relative to a corresponding control sweetener formulation that is identical to the standard formulation but lacks the plurality of amorphous silica particles.
[0262] Embodiment 101. The formulation of embodiment 100, wherein up to 40% of the caloric sweetener disposed in the individual sweetener particles is directly bound to the at least one amorphous silica particle.
[0263] Embodiment 102. The formulation of embodiment 100, wherein up to 30% of the caloric sweetener disposed in the individual sweetener particles is directly bound to the at least one amorphous silica particle.
[0264] Embodiment 103. The formulation of embodiment 100, wherein up to 20% of the caloric sweetener disposed in the individual sweetener particles is directly bound to the at least one amorphous silica particle.
[0265] Embodiment 103A. The formulation of any one of embodiments 100-103, further comprising any one of the limitations of embodiments 1-87, or any combination of the limitations.
[0266] Embodiment 104. A formulation comprising: (a) a first population of sweetener particles comprising a caloric sweetener and amorphous silica particles; (b) caloric sweetener particles; the caloric sweetener particles constitute at least 90% of the formulation by weight; The first population of sweetener particles contains the amorphous silica in an intra-particle weight ratio to the calorie sweetener in the range of 0.07:1 to 10:1; the total weight ratio of the total silica in the formulation to the total calorie sweetener in the formulation is in the range of 0.03% to 2% by weight; The formulation, wherein the caloric sweetener within the population of first sweetener particles is crystalline or exhibits crystalline behavior.
[0267] Embodiment 104A. The formulation of embodiment 104, wherein the caloric sweetener contains sucrose.
[0268] Embodiment 104B. The formulation of embodiment 104A, wherein the caloric sweetener contains at least 50% sucrose by weight.
[0269] Embodiment 104C. The formulation of embodiment 104A, wherein the caloric sweetener contains at least 65% sucrose by weight.
[0270] Embodiment 104D. The formulation of embodiment 104A, wherein the caloric sweetener contains at least 85% sucrose by weight.
[0271] Embodiment 104B. The formulation of embodiment 104A, wherein the caloric sweetener contains at least 95% sucrose by weight.
[0272] Embodiment 105. The formulation of any one of embodiments 104 to 104B, wherein the total weight ratio is in the range of 0.03% to 1.5%.
[0273] Embodiment 106. The formulation of embodiment 104, wherein the total weight ratio is in the range of 0.05% to 1.0%.
[0274] Embodiment 107. The formulation of embodiment 104, wherein the total weight ratio is in the range of 0.05% to 0.7%.
[0275] Embodiment 107A. The formulation of embodiment 104, wherein the total weight ratio is in the range of 0.05% to 0.5%.
[0276] Embodiment 108. The formulation of embodiment 104, wherein the total weight ratio is in the range of 0.05% to 0.35%.
[0277] Embodiment 109. The formulation of embodiment 104, wherein the total weight ratio is in the range of 0.05% to 0.25%.
[0278] Embodiment 110. The formulation of embodiment 104, wherein the total weight ratio is in the range of 0.05% to 0.2%.
[0279] Embodiment 111. A formulation according to any one of embodiments 104 to 110, wherein the total weight ratio is at least 0.07%.
[0280] Embodiment 112. A formulation according to any one of embodiments 104 to 110, wherein the total weight ratio is at least 0.085%.
[0281] Embodiment 113. A formulation according to any one of embodiments 104 to 110, wherein the total weight ratio is at least 0.10%.
[0282] Embodiment 114. A formulation according to any one of embodiments 104 to 107, wherein the total weight ratio is at least 0.5%.
[0283] Embodiment 115. A formulation according to embodiment 104 or embodiment 105, wherein the total weight ratio is at least 0.8%.
[0284] Embodiment 116. The formulation of embodiment 104, wherein the total weight ratio is at least 1.2%.
[0285] Embodiment 117. A formulation according to any one of embodiments 104 to 116, wherein the concentration of amorphous silica within the caloric sweetener particles is at most 0.1% by weight of the caloric sweetener particles.
[0286] Embodiment 118. The formulation of embodiment 117, wherein the concentration of amorphous silica within the caloric sweetener particles is at most 0.02% by weight of the caloric sweetener particles.
[0287] Embodiment 119. A formulation according to any one of embodiments 104 to 116, wherein the caloric sweetener particles constitute at least 95% of the formulation by weight.
[0288] Embodiment 120. The formulation of embodiment 119, wherein the caloric sweetener particles constitute at least 98% of the formulation by weight.
[0289] Embodiment 121. The formulation of embodiment 119, wherein the caloric sweetener particles constitute at least 99% of the formulation by weight.
[0290] Embodiment 122. The formulation of embodiment 119, wherein the caloric sweetener particles constitute at least 99.5% of the formulation by weight.
[0291] Embodiment 123. The formulation of any one of embodiments 104 to 122, wherein the intra-particle weight ratio is at least 0.10:1.
[0292] Embodiment 124. The formulation of embodiment 123, wherein the intra-particle weight ratio is at least 0.12:1.
[0293] Embodiment 125. The formulation of embodiment 123, wherein the intra-particle weight ratio is at least 0.15:1.
[0294] Embodiment 126. The formulation of embodiment 123, wherein the intra-particle weight ratio is at least 0.2:1.
[0295] Embodiment 127. The formulation of embodiment 123, wherein the intraparticle weight ratio is at least 0.25:1.
[0296] Embodiment 128. The formulation of embodiment 123, wherein the intraparticle weight ratio is at least 0.3:1.
[0297] Embodiment 129. The formulation of embodiment 123, wherein the intraparticle weight ratio is at least 0.5:1.
[0298] Embodiment 130. The formulation of embodiment 123, wherein the intraparticle weight ratio is at least 0.7:1.
[0299] Embodiment 131. The formulation of embodiment 123, wherein the intra-particle weight ratio is at least 1:1.
[0300] Embodiment 132. The formulation of embodiment 123, wherein the intraparticle weight ratio is at least 1.2:1.
[0301] Embodiment 133. The formulation of embodiment 123, wherein the intraparticle weight ratio is at least 1.5:1.
[0302] Embodiment 134. A formulation according to any one of embodiments 104 to 133, wherein the intra-particle weight ratio is at most 8:1.
[0303] Embodiment 135. A formulation according to any one of embodiments 104 to 133, wherein the intra-particle weight ratio is at most 4:1.
[0304] Embodiment 136. A formulation according to any one of embodiments 104 to 133, wherein the intra-particle weight ratio is at most 2.5:1.
[0305] Embodiment 137. A formulation according to any one of embodiments 104 to 133, wherein the intra-particle weight ratio is at most 1.5:1.
[0306] Embodiment 138. An edible formulation comprising: (a) a formulation according to any one of the preceding embodiments; and (b) at least one fat; (c) optionally at least one starch; The edible formulation, wherein the total concentration of all sweeteners, the at least one fat, and the at least one starch in the edible formulation is at least 30% by weight.
[0307] Embodiment 139. An edible formulation according to embodiment 138, wherein the weight content of all sweeteners in the edible formulation is at least 8%.
[0308] Embodiment 140. An edible formulation according to embodiment 138 or embodiment 139, containing at least 5% of all of said sweeteners and at least 5% of said at least one fat.
[0309] Embodiment 141. An edible formulation according to any one of embodiments 138 to 140, containing at least 5% of all of said sweeteners, and at least 5% of said at least one starch.
[0310] Embodiment 142. An edible formulation according to any one of embodiments 138 to 141, wherein the weight concentrations of all said sweeteners are within the range of 10% to 80%.
[0311] Embodiment 143. A method for producing the formulation of any one of embodiments 104 to 142, said method comprising: (a) forming a population of the first sweetener particles containing the caloric sweetener and the amorphous silica; (b) mixing the sweetener particles with the caloric sweetener particles.
[0312] Embodiment 144. The method of embodiment 143, wherein the caloric sweetener particles comprise sucrose.
[0313] Embodiment 145. The method of embodiment 143, wherein the caloric sweetener particles comprise primarily sucrose.
[0314] Embodiment 145A. The method of embodiment 143, wherein the caloric sweetener particles comprise at least 65% sucrose.
[0315] Embodiment 146. The method of embodiment 143, wherein the caloric sweetener particles are sucrose or regular table sugar.
[0316] Embodiment 147. A method for producing a food product, said method comprising: (a) providing a formulation according to any one of embodiments 1 to 103; and (b) mixing the sweetener particles with a caloric sweetener, such as a normal caloric sweetener, at least one fat, and optionally at least one starch.
[0317] Embodiment 148. The method of embodiment 147, wherein the total concentration of all sweeteners, the at least one fat, and the at least one starch in the food product is at least 30% by weight.
[0318] Embodiment 148A. The method of embodiment 147 or 148, wherein the caloric sweetener is a regular caloric sweetener.
[0319] Embodiment 149. The method of any one of embodiments 147 to 148A, wherein the mixing comprises mixing the sweetener particles with the at least one starch.
[0320] Embodiment 150. The method of any one of embodiments 147-149, wherein the sweetener comprises sucrose.
[0321] Embodiment 151. The method of any one of embodiments 147-149, wherein the sweetener comprises primarily sucrose.
[0322] Embodiment 152. The method of any one of embodiments 147 to 149, wherein the sweetener is sucrose.
[0323] As used herein, the term "sweetener carbohydrate" refers to a nutritive or caloric sweetener having at least one carbohydrate moiety, which is processed by the human body to produce energy. Sweetener carbohydrates produce a sweet taste when consumed by a typical human consumer. On a normalized sweetness scale, where maltose is approximately 0.31 and lactose is approximately 0.22, based on weight relative to sucrose, the term "sweetener carbohydrate" applies to lactose and any sugar or other nutrient carbohydrate-containing sweetener that has a sweetness between 0.15 and 2.5 on this normalized sweetness scale. Alternatively, the minimum sweetness of a sugar or other nutrient carbohydrate-containing sweetener may be stated to be that of raffinose (which has a sweetness of 0.15 on the scale). More typically, such sweetener carbohydrates have a sweetness within the ranges of 0.25 to 2.5, 0.35 to 2.5, 0.45 to 2.5, 0.25 to 1.8, 0.45 to 1.7, 0.15 to 1.7, or 0.35 to 1.5 on this normalized sweetness scale.
[0324] It is noted that the relative sweetness of fructose reported in the literature ranges from a minimum of 0.91 to a maximum of about 1.7. For the avoidance of doubt, the term "sweetening carbohydrate" is meant to include fructose regardless of any of its reported relative sweetness values.
[0325] As used herein, the term "normalized sweetness scale" refers to a weight-based relative sweetness scale in which sucrose is assigned a value of 1.00. More specifically, the normalized sweetness scale is determined according to the method disclosed in Moscowitz, H. "Ratio Scales of Sugar Sweetness"; Perception & Psychophysics, 1970, Vol. 7(5), in which the power functions of sugars and polyols / sugar alcohols as disclosed in Table 3 and provided herein below have an exponent of 1.3 (n=1.3). From "Ratio Scales of Sugar Sweetness" [Table 4]
[0326] The sweetener carbohydrate can be a monosaccharide or disaccharide. Examples of sweetener carbohydrates include, but are not limited to, sucrose, glucose, maltose, fructose, lactose, or any combination of sweetener carbohydrates. One or more sweetener carbohydrates can be combined with one or more sweetener polyols. The sweetener carbohydrate can be naturally occurring or synthetically produced.
[0327] As used herein, the term "sweetener polyol" refers to a consumable polyol that produces a sweet taste when consumed by a typical human consumer. Non-limiting examples of sweetener polyols include xylitol, maltitol, erythritol, sorbitol, threitol, arabitol, hydrogenated starch hydrolysate (HSH), isomalt, lactitol, mannitol, or galactitol (dulcitol). In many cases, polyols are sugar alcohols. Sugar alcohols can be produced from carbohydrates by any known reduction method (through chemical or biological conversion) of acids or aldehydes to alcohols. In other cases, sweetener polyols can be synthesized from parent carbohydrates. Alternatively, sweetener polyols can be obtained from biological sources.
[0328] For the avoidance of doubt, the term "sweetener polyol" is meant to include any polyol / sugar alcohol having a sweetness within the range of 0.15 to 2.5 on the above normalized sweetness scale. More typically, such sweetener polyols have a sweetness within the range of 0.15 to 1.5, 0.15 to 1.0, 0.15 to 0.8, 0.15 to 0.7, 0.20 to 0.7, 0.15 to 0.6, or 0.25 to 0.6 on this normalized sweetness scale.
[0329] The mean particle size (D50) is the number of particles in a population (D N50") or based on the particle volume (D V 50). These measurements can be obtained by a variety of known methods, including static light scattering (SLS), dynamic light scattering (DLS), sieving, and various methods of microscopy. Some methods may be preferred for a broader range of particles, while others may be preferred for a narrower range of particles.
[0330] As used herein and in the claims that follow, the term "specific surface area" refers to the Brunauer-Emmett-Teller (BET) method according to ISO standard 9277 for silica.
[0331] As used herein and in the claims that follow, the term "starch" is meant to include food starches that are or may be used in foods. Typically, such starches contain at least one of amylose and amylopectin, more typically both amylose and amylopectin. It will be understood that various modifications of starch can be made to impart specific chemical and / or physical properties to a particular food or to the starch in a particular food, including, by way of example, prevention of gelation at low temperatures, resistance to low pH, or resistance to high shear or temperature.
[0332] Starch is often present in ingredients, such as wheat flour. In white wheat flour, the starch content is usually about 68%. In oats, the starch content is usually about 58%.
[0333] In addition to including fats that are solid at room temperature (25°C), such as beef fat, shortening, palm oil, and butter, the term "fat," as used herein and in the claims that follow, is meant to include those that are liquid at room temperature, such as edible oils, including cooking oils. Specific examples of edible oils are olive oil, walnut oil, corn oil, and cottonseed oil.
[0334] The fat may be a separate ingredient or may be an ingredient within a food ingredient, for example, hazelnut paste and cocoa powder both contain fat.
[0335] As used herein and in the claims that follow, the term "conventional sweetener" refers to a caloric sweetener containing up to 0.08% amorphous silica, more typically up to 0.05%, up to 0.02%, or up to 0.01%. Even more typically, the conventional sweetener is a "standard" conventional sweetener that contains up to 0.005% amorphous silica on a dry weight basis, or is substantially devoid of or devoid of such amorphous silica.
[0336] Typically, conventional sweeteners are crystalline or exhibit crystalline behavior. "Canonical" conventional sweeteners are crystalline and always exhibit crystalline behavior.
[0337] As used herein and in the claims that follow, the term "conventional sugar" or the like refers to a conventional sweetener whose caloric sweetener content, on a dry weight basis, is at least 90% crystalline sucrose. More typically, the caloric sweetener content, on this dry weight basis, is at least 95%, at least 98%, or at least 99% crystalline sucrose.
[0338] For "conventional sweeteners" and "conventional sugars", the caloric sweetener content is at least 80%, more typically at least 90%, at least 95%, or at least 98%, by weight.
[0339] As used herein and in the claims that follow, the term "table sugar" refers to crystalline sucrose having a D50 (using sieve characterization or by other conventional means known to those skilled in the art) in the range of 300 to 1000 micrometers.
[0340] As used herein and in the claims that follow, the term "dissolution rate" refers to the dissolution rate as measured by the standard rate evaluation procedure provided in Examples 94 and 95.
[0341] As used herein and in the claims that follow, the term "identical" means, with respect to two formulations, that both the chemical composition and particle size distribution are substantially the same for the two formulations, as would be understood by one of ordinary skill in the art.
[0342] As used herein and in the claims that follow, the term "exhibiting improved sweetness" with respect to a formulation, such as a "standard formulation," refers to improved sweetness as determined by comparative sensory evaluation using the comparative sweetness index (minimum of 10 trained panelists) of Example 85. Typically, improved sweetness is evidenced by a CSI difference of at least 3, or at least 5, more typically at least 7, at least 10, at least 12, at least 15, or at least 20.
[0343] Comparative sensory evaluations are performed on either the standard formulation itself (compared to a corresponding control sucrose formulation identical to the standard formulation but lacking the plurality of amorphous silica particles) or the standard formulation incorporated into the Type II reduced sugar muffins, butter cookies, or hazelnut spreads of Examples 82B, 83A, and 84A. The corresponding control sucrose formulation identical to the standard formulation but lacking the plurality of amorphous silica particles is also incorporated into the same Type II reduced sugar muffins, butter cookies, or hazelnut spreads for comparative sensory evaluations.
[0344] As used herein and in the following claims, unless otherwise specified, the term "percent" or "%" refers to percent by weight. However, specifically in relation to a formulation containing silica and at least one sweetener, the weight percent of silica is relative to the sweetener. For example, in a formulation containing 1.3 grams of silica dispersed in a syrup containing 650 grams of sucrose and 350 grams of water, the weight percent of silica is 1.3 / 650=0.2%.
[0345] Similarly, the term "ratio," as used herein and in the claims that follow, refers to weight ratio, unless specifically indicated otherwise.
[0346] The modifiers "about" and "substantially" used in connection with quantities are inclusive of the stated value and have the meaning dictated by the context (e.g., they include at least the degree of error associated with measurement of the particular quantity). When used in conjunction with a particular value, that value should also be considered to be disclosed.
[0347] As used herein and in the claims that follow, the terms "primary," "predominantly," and the like, for example, with respect to sweeteners, refer to the sweetener having the highest concentration, by weight.
[0348] In the context of this application and the claims, the phrase "at least one of A and B" is equivalent to an inclusive "or" and includes any one of "A only," "B only," or "A and B." Similarly, the phrase "at least one of A, B, and C" is equivalent to an inclusive "or" and includes any one of "A only," "B only," "C only," "A and B," "A and C," "B and C," or "A and B and C."
[0349] It will be appreciated that certain features of the invention, which are, for clarity, described in the context of separate embodiments, may also be provided in combination in a single embodiment. Conversely, various features of the invention, which are, for brevity, described in the context of a single embodiment, may also be provided separately or in any suitable subcombination.
[0350] While the present invention has been described in conjunction with specific embodiments thereof, many alternatives, modifications, and variations will be apparent to those skilled in the art. Accordingly, it is intended to embrace all such alternatives, modifications, and variations that fall within the spirit and scope of the appended claims. All publications, patents, and patent applications mentioned in this specification are herein incorporated by reference in their entirety to the same extent as if each individual publication, patent, or patent application was specifically and individually indicated to be incorporated by reference. Furthermore, citation or identification of any reference in this application shall not be construed as an admission that such reference is available as prior art to the present invention.
Claims
1. 1. A formulation comprising: a population of first sweetener particles containing a plurality of amorphous silica particles within the population of first sweetener particles; Each individual sweetener particle of said sweetener particles comprises: (a) a low-calorie sweetener; (b) at least one amorphous silica particle disposed within each individual sweetener particle; the first population has an average particle size (Dv50-P) in the range of 20 to 1000 micrometers (μm); the average particle size (Dv50-S) of the plurality of amorphous silica particles is in the range of 0.8 to 20 micrometers (μm); an average ratio of the number of said plurality of amorphous silica particles to the number of said sweetener particles of at least 2.5:1; the population of first sweetener particles is less sweet than a control sweetener identical to the population of first sweetener particles but lacking the plurality of amorphous silica particles; The formulation, wherein when the first population is diluted with sucrose to produce a standard formulation containing 0.1% amorphous silica, the standard formulation exhibits improved sweetness relative to a corresponding control sucrose formulation identical to the standard formulation but lacking the plurality of amorphous silica particles.
2. 2. The formulation of claim 1, wherein each individual sweetener particle has a sweetener core devoid of the amorphous silica particles, the sweetener core having a diameter of at least 7 micrometers (μm), and the sweetener core is disposed at least 5 μm from the surface of each individual sweetener particle.
3. 3. The formulation of claim 2, wherein the diameter of the sweetener core is at least 40 μm.
4. 4. The formulation of claim 1, wherein the average ratio of the number of amorphous silica particles to the number of sweetener particles is at least 7:
1.
5. 10. A formulation according to any one of the preceding claims, wherein Dv50-P is at least 65 μm.
6. 10. A formulation according to any one of the preceding claims, wherein Dv50-S is at least 1 μm.
7. 10. The formulation of any one of the preceding claims, wherein a first weight ratio of the plurality of amorphous silica particles to the caloric sweetener is in the range of 0.07:1 to 10:
1.
8. 8. The formulation of claim 7, wherein the first weight ratio is at least 0.6:
1.
9. 10. The composition of claim 1, wherein within the first population, at least 50% by number of molecular units of the caloric sweetener are attached only to other molecular units of the caloric sweetener.
10. 10. A formulation according to any one of the preceding claims, wherein the sweetener formulation is in the form of a particulate solid.
11. 10. The formulation of any one of the preceding claims, wherein the conventional sweetener is a standard conventional sweetener.
12. 10. The formulation of any one of the preceding claims, wherein the difference in comparative sweetness index between the standard formulation and the corresponding control sucrose formulation that is identical to the standard formulation but lacks the plurality of amorphous silica particles is at least 3.
13. the population of first sweetener particles is the same as the population of second sweetener particles, but (i) devoid of said plurality of amorphous silica particles; (ii) A formulation according to any one of the preceding claims, which exhibits a slower dissolution rate relative to a control sweetener that is completely crystalline.
14. the population of first sweetener particles is the same as the population of second sweetener particles, but (i) devoid of said plurality of amorphous silica particles; (ii) A formulation according to any one of claims 1 to 13, which exhibits a slower dissolution rate relative to a control sweetener that is completely amorphous.
15. 15. The formulation of claim 13 or 14, wherein the dissolution rate of the first population of sweetener particles is at least 7% slower than the dissolution rate of the control sweetener.
16. 10. A formulation according to any one of the preceding claims, further comprising caloric sweetener particles.
17. the caloric sweetener particles constitute at least 90% of the formulation by weight; the first population of sweetener particles contains the amorphous silica particles in an intra-particle weight ratio to the caloric sweetener in the range of 0.07:1 to 10:1; the total weight ratio of the total silica in the formulation to the total calorie sweetener in the formulation is in the range of 0.03% to 2% by weight; 17. The formulation of claim 16, wherein the caloric sweetener within the first population of sweetener particles is crystalline or exhibits crystalline behavior.
18. 10. A formulation according to any one of the preceding claims, wherein the caloric sweetener contains at least 85% sucrose by weight.
19. 19. The formulation of any one of claims 16 to 18, wherein the concentration of amorphous silica within the caloric sweetener particles is at most 0.02% by weight of the caloric sweetener particles.
20. 20. The formulation of any one of claims 16 to 19, wherein the caloric sweetener particles comprise at least 95% of the formulation by weight.
21. A method for producing a formulation according to any one of claims 16 to 20, said method comprising: (a) forming a population of the first sweetener particles containing the caloric sweetener and the amorphous silica; (b) mixing the first population of sweetener particles with the caloric sweetener.
22. 1. A formulation comprising: (a) a formulation according to any one of claims 16 to 20; (b) at least one fat; (c) optionally at least one starch; 10. An edible composition wherein the total concentration of all sweeteners, said at least one fat, and said at least one starch in said composition is at least 30% by weight.
23. 23. The formulation of claim 22, wherein the weight concentration of all sweeteners is in the range of 10% to 80%.