Bulking agent for chocolate and other ingestibles
Processing non-cocoa plant seeds like grape seeds into cocoa extenders addresses the industry's challenge of finding cost-effective and flavorful alternatives to cocoa solids, achieving consistent chocolate quality and reduced variability.
Patent Information
- Application Number
- JP2025501556
- Authority / Receiving Office
- JP · JP
- Patent Type
- Applications
- Current Assignee / Owner
- Priority Date
- 2022-07-15
- Filing Date
- 2023-07-14
- Publication Date
- 2025-07-17
AI Technical Summary
The chocolate industry faces challenges in finding suitable alternatives for cocoa solids that maintain flavor and texture while reducing cost and variability, as existing extenders often impact flavor negatively and are difficult to process due to high fiber and lignin content.
Process non-cocoa plant seeds, such as grape seeds, through pH adjustment, roasting, and grinding to create a cocoa-like extender that mimics the properties of cocoa solids, including flavor and texture, using methods that reduce water content and particle size to match cocoa solids.
The processed plant seeds provide a cost-effective, flavorful, and consistent cocoa substitute that maintains the nutritional profile and processing functionality of traditional chocolate, reducing variability and enhancing flavor consistency.
Smart Images

Figure 2025523059000001_ABST
Abstract
Description
Technical Field
[0001] Cross - reference to Related Applications This application claims priority based on U.S. Provisional Application No. 63 / 389,483, filed on July 15, 2022. The disclosure of the prior application is considered to be a part of the disclosure of this application (incorporated into the disclosure of this application by reference).
[0002] Technical Field This document relates to methods and materials for processing non - cocoa plant seeds (e.g., grape seeds) and other non - cocoa plant parts and using them as extender ingredients for chocolate, cocoa, and other ingestible products.
Background Art
[0003] Background Generally, chocolate contains several basic components, cocoa butter, cocoa solids, and added sugar. Cocoa butter is the fat extracted from cocoa beans. Up to 50% of cocoa can be a fat containing both saturated fatty acids (e.g., palmitic acid and stearic acid) and monounsaturated acids (e.g., oleic acid). Cocoa butter provides the flavor and aroma of cocoa and is a major component of all types of chocolate. Dry cocoa solids are what remains after cocoa butter has been extracted from chocolate liquor (liquefied and ground cocoa beans). Untreated cocoa solids have a bitter and sour taste, but treatment of the cocoa with an alkaline agent (referred to as the "Dutch process" or "Dutching") to neutralize the acids can improve the flavor. Typically, as another basic component, sugar is added to chocolate. Cocoa beans contain a significant amount of carbohydrates, but most are in the form of starch and dietary fiber rather than sugar.
[0004] In some cases, chocolate may contain extenders to replace at least a portion of the cocoa solids. However, replacing cocoa solids can be a challenge as it is inherently difficult to reproduce the flavor in the final product. Their unique hydrophobic and high fiber properties are also not commonly found in easily commercialized food ingredients. When such properties are present in easily commercialized food ingredients, they often come with undesirable characteristics such as off-notes from oil and / or a high carbohydrate content. Attempts to isolate specific portions of cocoa solids have resulted in purified ingredients that lack complexity and are unsuitable as bulk substitutes for cocoa solids.
[0005] Current extenders include sugar, a small proportion of vegetable fat, and cheaper cocoa, but such extenders do not function well as 1:1 substitutes and may negatively impact the flavor of chocolate. For example, lupin has often been recommended as a chocolate substitute and has been commercially available as a fully purified bar product for decades. However, lupin lacks flavor compared to cocoa and has a disagreeable bean-like flavor that is very different from chocolate, so it has not been able to significantly replace cocoa. Attempts to manipulate the inherent properties of lupin have not resulted in a suitable product as a cocoa substitute.
[0006] Various extenders and coatings are also used in chocolate confectionery as substitutes for other cocoa-based ingredients. However, none of the existing chocolate extenders and compound coatings have successfully replaced the real dry cocoa solids in an ingestible chocolate product (which make up the majority of the body and substance of the cacao bean, the raw material of cocoa butter and cocoa solids). SUMMARY OF THE INVENTION
[0007] Summary The methods and materials provided herein take a new approach to creating cocoa extenders and coatings by addressing a long-standing need in the chocolate industry to find suitable alternatives for all or part of the dry cocoa solids in chocolate products. In particular, the methods and materials provided herein solve that problem by providing products and methods for producing padded chocolate in which all or part of the dry cocoa solids have been replaced with processed plant materials that are not derived from cocoa (e.g., fruit seeds such as grape seeds). Compositions containing the processed plant materials described herein are typically inexpensive (able to reduce cost and supply chain variability), able to maintain a strong cocoa flavor, and have few, if any, off-notes. In addition to having the aroma, flavor, smoothness, and body of premium chocolate, ingestibles made with the materials provided herein typically retain physical and chemical properties that are remarkably similar to those of traditional chocolate made from ground cacao beans. Further, the methods and materials disclosed herein can provide a high-fiber component that has a minimal impact on the nutritional profile of the finished product. For example, the processed plant materials provided herein do not share the macronutrient problems presented by some grains and / or sugars that are unsuitable as alternatives to cocoa solids due to their carbohydrate / sugar content.
[0008] As described herein, it has now been demonstrated that processed plant seeds (e.g., grape seeds, which are by-products of wine and juice production and are thus readily available) can be used to replace dry cocoa solids for chocolate, cocoa, padded chocolate, and other related products while in a dried, roasted, and / or pH-adjusted state. Further, surprisingly, it has been found that whole grape seeds, which are not currently used as food ingredients, are similar to whole cacao beans in their fiber and protein content (see Example 11).
[0009] The methods provided herein for processing plant seeds (e.g., non-cocoa fruit seeds such as grape seeds) successfully overcome several technical challenges. For example, grape seeds and other types of plant seeds (e.g., seeds of cranberry, blueberry, raspberry, strawberry, blackberry, pomegranate, date palm, and fenugreek) inherently have a very strong astringency due to their high tannin content. In fact, due to the strong astringency of grape seeds, the top priority when pressing grapes to make wine is to prevent the destruction of the seeds so that the high levels of tannins contained in the seeds do not mix into the grape juice. The pH adjustment, roasting, and temperature treatment steps in the methods provided herein can help regulate and manipulate the tannin profile of grape seeds. Another challenge is that grape seeds and other types of plant seeds (e.g., cranberry seeds, blueberry seeds, raspberry seeds, strawberry seeds, blackberry seeds, pomegranate seeds, date palm seeds, and fenugreek seeds) are typically difficult to grind due to their high content of lignin and liquid oil. Lignans are abundantly found in grape seeds, berry seeds, and other plants and are concentrated in the cell walls of the seeds. The grinding techniques used in the methods provided herein can address this problem and result in particles of a size similar to finely ground dry cocoa solids. One advantage of grinding tough, fibrous, high-lignin seeds is that the bioavailability of the beneficial compounds contained in the lignin can be improved. For example, when berry seeds are consumed whole without being crushed, it has been found that the bioavailability of lignin is relatively low because the seeds pass through the intestine and most of the lignin content is lost.
[0010] Yet another problem is that the flavors of grape seeds and other non-cocoa plant seeds are not inherently cocoa-like. However, the methods provided herein for processing seeds including grape seeds, cranberry seeds, raspberry seeds, blackberry seeds, pomegranate seeds, and strawberry seeds can result in products having a desired cocoa flavor and reduced off-flavors. For example, refer to the results described in Example 12 herein, which demonstrate that the aforementioned seeds, although not inherently cocoa-like, acquire a cocoa flavor after being processed as described herein.
[0011] It should be noted that the approach described herein for converting non-cocoa plant seeds into a cocoa substitute is different from the general approaches taken in the food industry to create alternative products or substitutes for natural ingredients or products. Generally, the approach used in the food industry is to purify food products in order to eliminate, to the extent possible, different colors, odors, and textures. For example, margarine is a refined, bleached, deodorized fat that is manipulated to have the texture of butter made from milk and is mixed with flavors and colorings added to mimic butter made from milk. In contrast, the materials and methods described herein were identified and developed by investigating various natural food ingredients in order to identify similar qualities, rather than synthesizing a mimicking product from the start. Since fruit seeds were identified as candidates, methods were developed for processing the seeds into a product closely resembling cocoa.
[0012] This book provides materials and methods for using plant seeds (e.g., non-cacao plant seeds such as grape seeds and berry seeds) or other plant parts as an extender ingredient in chocolate, cocoa, or other ingestible products. The processing methods provided herein can include, without limitation, steps of pH adjustment, roasting, and / or grinding to produce extender products having a surprisingly accurate cocoa-like flavor, as demonstrated in the descriptive sensory tests described in Example 8 herein compared to authentic chocolate. The results of the sensory tests demonstrated that substitution with a processed grape seed extender at 75 wt% dry cocoa solids results in a chocolate product indistinguishable from authentic chocolate.
[0013] The plant-based (e.g., seed-based) extenders provided herein can be used in a dried, roasted, and / or pH-adjusted state. The use of such extenders can reduce the cost of the final product containing chocolate or cocoa, can reduce the variability in the price of the finished product (which can occur due to changes in climate conditions, labor issues, regional political policies, etc.), can increase the flexibility of chocolate and cocoa manufacturers to maintain consistency in flavor from season to season as a blending tool, and can enhance the processing functionality of liquid chocolate.
[0014] In a first aspect, the present book features a composition containing roasted and ground fruit seeds or consisting essentially of roasted and ground fruit seeds. In some cases, the ground fruit seeds have a particle size of less than 350 microns. The fruit seeds can be grape seeds. The grape seeds can be selected from table grapes, Concord, Niagara, Chardonnay, Sauvignon Blanc, Muscat, Sultana, Riesling, Pinot Grigio, Pinot Gris, Cabernet Sauvignon, Merlot, Pinot Noir, Shiraz, Albariño, Malbec, Grüner Veltliner, Solaris, Zinfandel, Cabernet Franc, Tempranillo, Carmenère, Mataro, Sangiovese, Regent, Black Muscat, Chasselas, wild grape, Nebbiolo, Montepulciano, Gewürztraminer, Barbera, Schönburger, Carignan, Semillon, Gamay, Petit Verdot, Trebbiano, Sancerre, Grüner Veltliner, Silvaner, Petit Syrah, Grüner Veltliner Blanc grapes, and any combination thereof. In some cases, the fruit seeds can be selected from cranberries, raspberries, blueberries, strawberries, blackberries, pomegranates, kiwis, watermelons, musk melons, cantaloupes, honeydews, papayas, passion fruits, star fruits, tomatoes, tomatillos, dragon fruits, guavas, loquats, calamansi, pumpkins, squashes, okras, cucumbers, bell peppers, eggplants, peaches, apples, cherimoyas, pineapples, quince, loquats, dates, fenugreek, and any combination thereof. The ground fruit seeds have a particle size of less than 250 microns or less than 150 microns.
[0015] In another aspect, the present book features an ingestible product containing roasted and ground fruit seeds or an extender substantially consisting of roasted and ground fruit seeds. In some cases, the ground fruit seeds have a particle size of less than 350 microns. The ingestible product can be chocolate. The chocolate can contain from about 0.01% to about 35% by weight of the extender; from about 20% to about 55% by weight of cocoa butter; from about 20% to about 60% by weight of sugar; and optionally from about 0.5% to about 25% by weight of cocoa solids. In some cases, the chocolate can contain about 17.5% by weight of the extender; about 37.5% by weight of cocoa butter; about 40% by weight of sugar; and optionally about 5% by weight of cocoa solids.
[0016] The fruit seeds can be grape seeds. The grape seeds can be selected from table grapes, Concord, Niagara, Chardonnay, Sauvignon Blanc, Muscat, Sultana, Riesling, Pinot Gris, Pinot Grigio, Cabernet Sauvignon, Merlot, Pinot Noir, Shiraz, Albariño, Malbec, Grüner Veltliner, Solaris, Zinfandel, Cabernet Franc, Tempranillo, Carmenère, Mataro, Sangiovese, Regent, Black Muscat, Chasselas, wild grape, Nebbiolo, Montepulciano, Gewürztraminer, Barbera, Schönburger, Carignan, Semillon, Gamay, Petit Verdot, Trebbiano, Sancerre, Grüner Veltliner, Silvaner, Petit Syrah, Grüner Veltliner Blanc grapes, and any combination thereof. In some cases, the fruit seeds can be derived from cranberries, raspberries, blueberries, strawberries, blackberries, pomegranates, kiwis, watermelons, honeydews, cantaloupes, papayas, passion fruits, star fruits, tomatoes, tomatillos, dragon fruits, guavas, loquats, calamansi, pumpkins, squashes, okras, cucumbers, bell peppers, eggplants, pears, apples, cherimoyas, pineapples, quince, loquats, dates, fenugreek, and any combination thereof. The ground fruit seeds have a particle size of less than 250 microns or less than 150 microns.
[0017] In one aspect, the present book features a method for producing a substitute for dry cocoa solids from non-cocoa seeds, where the method includes: (a) a step of treating a number of non-cocoa fruit seeds with a chemical solution and / or an enzyme solution, thereby producing treated seeds; (b) a step of reducing the water content of the treated seeds to 25% w / w or less of the treated seeds, thereby producing dried seeds; (c) a step of roasting the dried seeds, thereby producing roasted seeds; and (d) a step of grinding the roasted seeds, thereby producing a ground seed composition that is effective as a substitute for dry cocoa solids.
[0018] In another aspect, the present book features a method for producing a chocolate product containing a bulking agent prepared from non-cocoa seeds, where the method includes: (a) a step of treating a number of non-cocoa fruit seeds with a chemical solution and / or an enzyme solution, thereby producing treated seeds; (b) a step of reducing the water content of the treated seeds to 25% w / w or less of the treated seeds, thereby producing dried seeds; (c) a step of roasting the dried seeds, thereby producing roasted seeds; and (d) a step of grinding the roasted seeds, thereby producing a ground seed composition that is used as all or part of a bulking agent.
[0019] In some cases, a number of non-cocoa fruit seeds are washed to remove impurities such as husks, broken materials, stones, skins, stems, and / or branches before step (a). The number of non-cocoa fruit seeds can be washed using a destoner, scalping deck, suction channel, sizing deck, optical sorter, sieve, or a combination thereof such that the impurities are less than 0.5% w / w of the seeds.
[0020] In some cases, step (a) involves using a chemical solution containing a caustic agent (e.g., sodium hydroxide, potassium hydroxide, sodium carbonate, calcium carbonate, calcium hydroxide, potassium bicarbonate, iodine, or a combination thereof), an acidulant (e.g., acetic acid, adipic acid, citric acid, fumaric acid, lactic acid, malic acid, phosphoric acid, and tartaric acid, glucono delta lactone, or a combination thereof), and / or an oxidizing agent (e.g., hydrogen peroxide). The seeds can be treated with the chemical solution at 60°C to 150°C (e.g., 75°C to 100°C) for 30 minutes to 2 hours while stirring so that the treated seeds have a pH of 5.5 to 10.5 (e.g., 8 to 10). In some cases, step (a) involves using an enzyme solution containing one or more enzymes including cellulase, tannase, pectinase, xylanase, and / or hemicellulase, preferably cellulase and / or hemicellulose, in an aqueous solution. The seeds can be treated with the enzyme solution for 30 minutes to 2 hours while stirring.
[0021] In some cases, step (a) involves treating the seeds with the chemical solution and / or the enzyme solution by immersion, spraying, boiling, stirring, coating, or a combination thereof. In some cases, step (a) involves treating the seeds with both the chemical solution and the enzyme solution simultaneously or sequentially.
[0022] In some cases, step (b) involves reducing the water content of the treated seeds to 20% w / w, 15% w / w, 10% w / w, 6% w / w, or less of the treated seeds.
[0023] In some cases, step (c) involves roasting the dried seeds at 125°C to 200°C, preferably 140°C to 200°C, or 150°C to 175°C for 20 minutes to 2 hours. The water content of the roasted seeds can be less than 2% w / w of the roasted seeds.
[0024] In some cases, step (d) includes using one or more dry milling techniques and / or one or more wet milling techniques to produce a ground seed composition. In some cases, step (d) includes using a wet mill (e.g., a stone mill, a colloid mill, a blade mill, or a corundum mill) to grind the roasted seeds with a fat or a liquid oil. The fat or liquid oil can be in an amount of 30 to 60% by weight of the roasted seeds. In some cases, step (d) includes grinding the roasted seeds to a particle size of less than about 350 μm, less than about 250 μm, or less than about 150 μm.
[0025] In one aspect, the present book features a method for manufacturing a substitute for dry cocoa solids from non-cocoa seeds, where the method includes: (a) a step of washing a number of non-cocoa fruit seeds to remove impurities, thereby producing washed seeds; (b) a step of roasting the washed seeds at 125°C to 200°C, preferably 140°C to 200°C, for 20 minutes to 2 hours, thereby producing roasted seeds; and (c) a step of grinding the roasted seeds, thereby producing a ground seed composition that is effective as a substitute for dry cocoa solids. In another aspect, the present book features a method for manufacturing a chocolate product containing an extender prepared from non-cocoa seeds, where the method includes: (a) a step of washing a number of non-cocoa fruit seeds to remove impurities, thereby producing washed seeds; (b) a step of roasting the washed seeds at 125°C to 200°C, preferably 140°C to 200°C, for 20 minutes to 2 hours, thereby producing roasted seeds; and (c) a step of grinding the roasted seeds, thereby producing a ground seed composition that is used as all or part of the extender. In some cases, the method further includes reducing the water content of the washed seeds before step (b). In some cases, step (c) includes using a wet grinder (e.g., a stone mill, a colloid mill, a blade mill, or a corundum mill) to grind the roasted seeds together with a fat or a liquid oil, where the fat or the liquid oil is in an amount of 30 to 60% by weight of the roasted seeds. In some cases, step (d) includes grinding the roasted seeds to a particle size of less than about 350 μm, less than about 250 μm, or less than about 150 μm.
[0026] In some cases, the chocolate products described herein further include cocoa butter, sugar, and optionally cocoa solids. In some cases, the chocolate products described herein further include a cocoa butter alternative, substitute, or equivalent (CBE), sugar, and optionally cocoa solids, seed meal, and / or lecithin.
[0027] As used herein, the terms "traditional" or "reference" with respect to chocolate refer to chocolate products made by standard chocolate manufacturing processes and containing standard chocolate ingredients including cocoa solids, cocoa butter, and sugar.
[0028] As used herein, the term "about", when used to refer to the amount of a component or compound in chocolate or other ingestible products, means ±10% of that amount. As used herein, the term "about", when used to refer to a measured characteristic of chocolate or other ingestible products, means ±20% of the reported value. As used herein, the term "about", when used in connection with the conditions for manufacturing chocolate or other ingestible products, means ±20% of that value.
[0029] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains. Although methods and materials similar or equivalent to those described herein can be used to practice the invention, suitable methods and materials are described below. All publications, patent applications, patents, and other references mentioned herein are incorporated by reference in their entirety. In case of conflict, the present specification, including definitions, will control. Furthermore, the materials, methods, and examples are illustrative only and not intended to be limiting.
[0030] Details of one or more aspects of the present invention are set forth in the accompanying drawings and the description below. Other features, objects, and advantages of the invention will be apparent from the specification and claims.
Brief Description of the Drawings
[0031]
Figure 1
Figure 2
Modes for Carrying Out the Invention
[0032] Detailed Description This document provides materials and methods for using plant seeds (e.g., grape seeds) and / or other plant parts as raw materials for extender components that can be used for the increment of chocolate, cocoa, or other ingestible products. For example, in chocolate, all or a portion of the cocoa solids can be replaced with the extenders provided herein. Plant-based (e.g., seed-based) extenders can be used in a dried, roasted, and / or pH-adjusted state. The use of such extenders can reduce the cost of the final product containing chocolate or cocoa, can reduce the variability in the price of the finished product (which can occur due to changes in climate conditions, labor issues, and political policies in the growing regions), can increase the flexibility of chocolate and cocoa manufacturers for maintaining flavor consistency seasonally as a blending tool or cocoa replacement tool, and can enhance the processing functionality of liquid chocolate. The extenders provided herein are typically not derived from cacao / cocoa (e.g., do not contain cacao solids or cocoa solids). The extenders can be prepared, for example, from food stream waste (e.g., seeds, stems, leaves, etc.).
[0033] In some aspects, the present document provides bulking agents that can be used in chocolate and other ingestibles. The bulking agents can be made, for example, from food stream waste. For example, the bulking agents can include processed seeds (e.g., grape seeds or seeds derived from any other suitable type of plant). Grape seeds can be useful for a variety of reasons. For example, the fiber and protein content of grape seeds is similar to that of cacao beans on a solid basis. Grape seeds grow in a high acid, high sugar pulp similar to cacao beans (grapes and pods), which can result in a similar composition of flavor precursors.
[0034] For example, after evaluating multiple plants and food raw materials (e.g., seeds, grains, roots, fruits, and vegetables), it was identified that both cocoa beans (cocoa seeds) and grape seeds are seeds with extremely high tannin content, and it was discovered that this property can be manipulated for flavor and mouthfeel purposes. Details of the high tannin content of cocoa beans (cocoa seeds) and grape seeds can be found, for example, in Mohd Z.N., et al. (2020). Microanalysis of Cocoa Beans for Determination of Tannin Content Contributed to Cocoa Flavor. Malaysian Cocoa Journal 12(1):154-161; and Ma Z.F., et al. Phytochemical Constituents, Health Benefits, and Industrial Applications of Grape Seeds: A Mini-Review. Antioxidants (Basel). 2017 Sep 15;6(3):71, each of which is hereby incorporated by reference in its entirety. Furthermore, studies have shown that both grape seeds and cocoa beans have a high flavonoid content that can be beneficial for human health. Details of the high flavonoid content of grape seeds and cocoa beans can be found, for example, in Ma Z.F., et al. Phytochemical Constituents, Health Benefits, and Industrial Applications of Grape Seeds: A Mini-Review. Antioxidants (Basel). 2017 Sep 15;6(3):71; and Katz D.L., et al. Cocoa and chocolate in human health and disease. Antioxid Redox Signal. 2011 Nov 15;15(10):2779-811, each of which is hereby incorporated by reference in its entirety.
[0035] Typically, lignans, a group of bioactive compounds concentrated in plant seeds, are also present in significant amounts. Lignans are associated with a wide range of health-promoting effects such as antioxidant, antiviral, and antitumor effects. Details of lignans can be found, for example, in Smeds, A., et al. (2012). Content, composition, and stereochemical characterisation of lignans in berries and seeds. Food Chemistry. 194. 1991, which is hereby incorporated by reference in its entirety.
[0036] Furthermore, from a production perspective, grape seeds are by-products of wine and juice production and are thus readily available as ingredients. They are typically treated as waste, and according to some estimates, about 10 - 12 kg of grape seeds per 100 kg of wet residue are produced by the wine industry. Therefore, grape seeds are a relatively inexpensive source of healthy dietary fiber and lignans rich in antioxidants, reaching 38 - 52% on a dry matter basis. Details can be found, for example, in Ma Z.F., et al. Phytochemical Constituents, Health Benefits, and Industrial Applications of Grape Seeds: A Mini-Review. Antioxidants (Basel). 2017 Sep 15;6(3):71, which is hereby incorporated by reference in its entirety. Additionally, vineyards often have long-term planting plans in areas where there was previously little vegetation, and thus the use of grape seeds as a substitute for cocoa beans poses a lower deforestation risk.
[0037] Furthermore, it has been discovered here that processed grape seeds have several desirable traits, including rheological properties (e.g., viscosity), a cocoa-like chemical profile upon roasting, and the ability to be ground into a refined paste with an appropriate particle size. As noted above, grape seeds surprisingly have characteristics similar to cocoa seeds. For example, grape seeds retain hydrophobicity, a high fiber / cellulose content that mimics the reaction of cocoa to processing. That is, the extender provided herein can be substituted where cocoa solids are normally used, both in primary manufacturing formulations and in consumer applications such as chocolate products, beverages, confections, etc. for baking. Since the seeds can be milled to a cocoa-like fine particle size, the extender has a consistent smoothness that cannot be perceived by the human tongue. The characteristic of a fine particle size (e.g., less than 40 microns, less than 35 microns, or even less than 25 microns) can be an important indicator of chocolate quality. Furthermore, grape seeds can be consistently processed and their color can be adjusted to match the color of cocoa solids. In particular, grape seeds can be discolored to a dark brown by roasting and the color can be darkened by pH adjustment, similar to adjusting the coloring of cocoa powder. Additionally, the seeds have a low viscosity and yield value compared to cocoa solids. This is a surprisingly beneficial discovery as it means that processed grape seed products have improved flow characteristics compared to traditional dry cocoa solids and reduces the need for unnecessary yield value regulating ingredients such as polyglycerol polyricinoleate (PGPR) in chocolate formulations containing the extender provided herein.
[0038] Seeds derived from any suitable type of grape can be used. The types of grape seeds that can be used to produce the bulking agent described herein include, without limitation, table grapes, Concord, Niagara, Chardonnay, Sauvignon Blanc, Muscat, Sultana, Riesling, Pinot Grigio, Pinot Gris, Cabernet Sauvignon, Merlot, Pinot Noir, Shiraz, Albariño, Malbec, Grüner Veltliner, Solaris, Zinfandel, Cabernet Franc, Tempranillo, Carmenère, Mataro, Sangiovese, Regent, Black Muscat, Chasselas, wild grapes, Nebbiolo, Montepulciano, Gewürztraminer, Barbera, Chenin Blanc, Carignan, Semillon, Gamay, Petit Verdot, Trebbiano, Sémillon, Grüner Veltliner, Sylvaner, Petit Syrah, and seeds derived from grapes of Grüner Veltliner Blanc. Combinations of seeds from two or more types of grapes can also be used. Since grape seeds are often obtained as waste from wineries and juice manufacturers, seed lots can contain combinations of grape seeds of different varieties. Any combination of grape seeds derived from any combination of grape types can be used.
[0039] It should be noted that fruits and vegetable seeds other than grape seeds can also be used in the bulking agents and methods provided herein. For example, but not limited to, seeds derived from cranberries, raspberries, blueberries, strawberries, blackberries, pomegranates, cloudberries, kiwis, watermelons, honeydews, cantaloupes, honeydews, papayas, passion fruits, star fruits, tomatoes, cherry tomatoes, dragon fruits, guavas, prickly pears, calamansi, pumpkins, squashes, okras, cucumbers, peppers, eggplants, pears, apples, cherimoyas, pineapples, quinces, loquats, dates, and fenugreek can be used. Fruit seeds, including seeds of all berries, are by-products of berry processing and are therefore relatively inexpensive and readily available as food stream waste. For example, most berries, including cranberries, raspberries, blueberries, and cloudberries, are utilized in the food industry for juice production, and the pressing of berries results in the production of large amounts of berry processing waste, including the skins, seeds, and stems of the berries, which can account for approximately one-quarter of the total mass of the berries. Details can be found, for example, in Alba, K., et al. (2019). Dietary Fibre from Berry-Processing waste and its impact on bread structure: a review. Journal of the Science of Food and Agriculture. 99. 10. 1002 / jsfa.9633, which is hereby incorporated by reference in its entirety. Combinations of seeds from two or more fruits may be used. Fruit seeds, such as berry seeds, are often obtained as waste from juice manufacturers and fruit processors, so seed lots may contain combinations of different types of fruit seeds, including combinations of berry seeds. Any combination of fruit seeds derived from any combination of fruit raw materials can be used.
[0040] As demonstrated herein, fruit seeds other than grape seeds also gave results similar to those of grape seeds. In particular, Example 12 describes data from a sensory evaluation conducted using various fruit seeds processed according to the same methods described herein for grape seeds and milled to a particle size of about 40 microns or less. As described in Example 12, substitutes for dry cocoa solids were successfully produced using seeds derived from raspberries, blackberries, cranberries, blueberries, strawberries, and pomegranates. The seeds of dates and fenugreek were also tested and gave desirable results.
[0041] In some cases, the bulking agent provided herein can be food waste in which most (e.g., at least 75 wt%, at least 80 wt%, at least 85 wt%, at least 90 wt%, or at least 95 wt%) of the starch, protein, sugar, fat-soluble components, and flavor has been removed and cellulose, hemicellulose, lignin, and / or other insoluble fibers remain. In some embodiments, the solid substrate can include processed or unprocessed grains or grain products, legumes or legume seeds, oilseed plants or oilseed seeds, fruits or fruit products, roots, tubers, or products of roots or tubers, sugar processing by-products, or other plant by-products.
[0042] In some cases, the extender may include processed or unprocessed grains. Processing of the grains can result in the removal or partial removal of one or more of starch, protein, sugar, fat-soluble components, and flavor. Non-limiting examples of grains and grain products that can be used as extenders include atella, barley distillers by-products, broken or polished rice, barley grains, brown rice, beer lees, Echinochloa crusgalli grains, corn gluten feed, corn distillers grains, corn gluten meal, ear maize, Eleusine coracana grains, Setaria italica grains, Digitaria exilis grains, maize bran or hominy feed, maize green forage, maize cobs, maize stover, maize germ meal or maize germ, malt culms, maize grains, millet hulls, oat hulls or oat mill feed, oats, Pennisetum glaucum grains, Panicum miliaceum grains, Chenopodium quinoa, Avena sativa grains, rice protein concentrate, rice bran, or other rice by-products, paddy rice, rice husks, rye grains or by-products, sorghum by-products, starch, sorghum grains, Eragrostis tef grains, triticale, Paspalum fasciculatum, wheat (in general), wheat germ, wheat bran, wheat grains, wheat distillers grains, wheat shorts, wheat middlings, wheat feed flour, and mixtures thereof.
[0043] In some cases, the bulking agent can be prepared from leguminous plants or leguminous plant seeds. Non-limiting examples of leguminous plants or leguminous plant seeds that can be used as substrates include African locust bean (Parkia biglobosa or Parkia filicoidea), African yam bean (Sphenostylis stenocarpa), crop residues and straw of Bambara groundnut (Vigna subterranea), black gram (Vigna mungo), pods, husks, and residues of Bambara groundnut (Vigna subterranea), blue lupin (Lupinus angustifolius) seeds, Bambara groundnut (Vigna subterranea) seeds, butterfly pea (Clitoria ternatea), carob (Ceratonia siliqua), common bean (Phaseolus vulgaris), centro (Centrosema molle), common vetch (Vicia sativa), chickpea (Cicer arietinum), cowpea (Vigna unguiculata) seeds, broad bean (Vicia faba), grass pea (Lathyrus sativus), guar (Cyamopsis tetragonoloba) forage, seeds, and meal, guanacaste (Enterolobium cyclocarpum), hairy vetch (Vicia villosa), horse gram (Macrotyloma uniflorum), jack bean (Canavalia ensiformis), lablab (Lablab purpureus), lima bean (Phaseolus lunatus), lentil (Lens culinaris), mat bean (Vigna aconitifolia), mung bean (Vigna radiata), Narbonne vetch (Vicia narbonensis), pea by-products, peanut seeds, pea protein concentrate, peanut skins, pea seeds, pigeon pea (Cajanus cajan) seeds, peanut forage, prickly sesban (Sesbania bispinosa), peanut hulls, purple vetch (Viciabenghalensis), peanut meal, Albizia saman, Vigna umbellata, Sesbania sesban, soybean seeds, soybeans (in general), Canavalia gladiata, soybean forage, Prosopis farcta, soybean meal, Tamarindus indica, Prosopis tamarugo, Mucuna pruriens, Lupinus albus seeds, Psophocarpus tetragonolobus, Lupinus luteus seeds, and mixtures thereof are included.
[0044] In some cases, the extender can be prepared from oilseed plants or oilseeds, or a combination of one or more oilseed plants and / or one or more oilseeds. Non-limiting examples of oilseed plants or oilseeds that can be used include almond kernels and by-products, Argania spinosa, Attalea speciosa, Shorea stenoptera oil meal, Bactris gasipaes, Camelina sativa seeds and oil meal, cotton (in general), Anacardium occidentale nuts and by-products, Ricinus communis seeds, oil meal, and by-products, cotton straw and cotton crop residues, Mesua ferrea, chia seeds, cocoa butter, cottonseed hulls, cottonseed meal, copra meal and coconut by-products, Crambe abyssinica, Attalea cohune seeds and oil meal, Hyphaene thebaica, Lallemantia iberica, flax straw and flax crop by-products, grape seeds and grape seed oil meal, hemp, Jatropha sp.)Kernel meal and other Jatropha products, jojoba (Simmondsia chinensis), kapok (Ceiba pentandra), kenaf (Hibiscus cannabinus), karanja (Millettia pinnata), kusum (Schleichera oleosa), linseed meal, loofah (Luffa aegyptiaca), flax, macadamia (Macadamia integrifolia), moringa (Moringa oleifera), madhuca (Madhuca longifolia), mustard oil meal and mustard bran, maize germ meal and maize germ, neem (Azadirachta indica), niger (Guizotia abyssinica), coconut leaves and coconut crop residues, olive oil cake and by-products, coconut kernel, coconut kernel meal, peanut seeds, palm oil mill effluent, peanut skins, coconut compressed fiber, pinto peanut (Arachis pintoi), peanut forage, poppy (Papaver somniferum), peanut hulls, pumpkin, squash, gourds, and other Cucurbita seeds, peanut meal, rapeseed forage, rapeseed hulls, rapeseed meal, rapeseed, rubber (Hevea brasiliensis), safflower (Carthamus tinctorius) seeds and oil meal, sal (Shorea robusta) seeds and oil meal, soybean meal, soybean seeds, oenocarpus (Oenocarpus bataua), sunflower (general), sesame (Sesamum indicum) seeds and oil meal, shea butter, shea kernel, sickle pods, sunflower forage and crop residues, sunflower hulls and sunflower fines, sunflower meal, sunflower seeds, soybeans (general), soybean forage, soybean hulls, tung (Aleurites fordii), tomato seed cake, walnut (Juglans regia), watermelon (Citrullus lanatus) seeds and oil meal, and mixtures thereof are included.
[0045] In some cases, the extender can be prepared from fruits or fruit products. Non-limiting examples of fruits and fruit products that can be used include apple pomace and inferior apples, banana (in general), banana peel, banana fruit, banana leaves and pseudostems, breadnut (Artocarpus altilis), breadnut tree (Brosimum alicastrum), cashew (Anacardium occidentale) nuts and by-products, citrus fresh pulp, citrus fruits, citrus seed meal, citrus molasses, citrus dried pulp, colocynth (Citrullus colocynthis), date palm molasses, date palm leaves and date palm pedicels, date palm fruits, grape pomace, guava (Psidium guajava), grape seeds and / or grape seed oil meal, jackfruit (Artocarpus heterophyllus), kokum (Garcinia indica), loofah (Luffa aegyptiaca), mango (Mangifera indica) fruits and by-products, moringa (Moringa oleifera), melon (Cucumis melo), olive oil cake and by-products, papaya (Carica papaya) fruits, leaves, and by-products, pineapple by-products, pineapple leaves, pineapple juice, pumpkin, squash, gourds, and other cucurbitaceae species, paradise nut tree (Lecythis pisonis), mamoncillo (Melicoccus bijugatus), seje (Oenocarpus bataua), tomato fruits, tomato pomace, tomato peels and tomato seeds, tomato leaves and crop residues, tomato seed cake, walnut (Juglans regia), watermelon (Citrullus lanatus) forage and fruits, watermelon (Citrullus lanatus) seeds and oil meal, and mixtures thereof. In some embodiments, the solid substrate includes grape seeds.
[0046] The bulking agent can also be prepared from roots, tubers, and products of roots or tubers. Non-limiting examples of roots, tubers, and products of roots or tubers that can be used include arrowroot (Maranta arundinacea), sugar beet pulp, canna (Canna indica), carrot (Daucus carota), cassava leaves and foliage, cassava peel, cassava pomace, and other cassava by-products, cassava roots, Chinese yam (Dioscorea esculenta), ensete (Ensete ventricosum) corms and pseudostems, fodder beet roots, maca, Jerusalem artichoke (Helianthus tuberosus), cocoyam (Xanthosoma sagittifolium), potato (Solanum tuberosum) by-products, potato (Solanum tuberosum) tubers, sugar beet dehydrated pulp, sugar beet compressed or non-dehydrated pulp, sugar beet roots, sugar beet tops, sweet potato (Ipomoea batatas) by-products, sweet potato (Ipomoea batatas) forage, sweet potato (Ipomoea batatas) tubers, taro (Colocasia esculenta), white yam (Dioscorea rotundata), greater yam (Dioscorea alata), elephant foot yam (Amorphophallus campanulatus), yacon (Smallanthus sonchifolius), yellow yam (Dioscorea cayenensis), and mixtures thereof.
[0047] In some cases, the bulking agent can be prepared from sugar processing by-products. Non-limiting examples of sugar processing by-products that can be used include sugar beet pulp, sugar, molasses, sugar beet compressed or non-dehydrated pulp, sugarcane bagasse, sugarcane forage, whole plants, sugarcane juice, sugarcane molasses, sugarcane press mud, sugarcane tops, and mixtures thereof.
[0048] Other plant by-products that can be used to prepare the extender include, without limitation, carob (Ceratonia siliqua), citrus molasses, date palm molasses, date palm leaves and fronds, date palm seeds, the corms and pseudostems of ensete (Ensete ventricosum), leaf protein concentrate and grass juice, Mexican marigold (Tagetes erecta), mushrooms and spent mushroom substrate, molasses / urea blocks, potato (Solanum tuberosum) tubers, Jerusalem artichoke press cake, spent hops, straw, sugarcane juice, sugarcane molasses, sugarcane press mud, vinasse, wood, wood sugar, or wood molasses, and mixtures thereof.
[0049] This document also provides a method for manufacturing the extender. The extender provided herein can be prepared using any suitable method.
[0050] In some cases, the extender can be prepared using ground plant seeds as starting materials. For example, ground seeds (e.g., ground grape seeds, cranberry seeds, raspberry seeds, blackberry seeds, strawberry seeds, blueberry seeds, pomegranate seeds, kiwi seeds, watermelon seeds, muskmelon seeds, cantaloupe seeds, honeydew seeds, papaya seeds, passion fruit seeds, star fruit seeds, tomato seeds, cherry tomato seeds, dragon fruit seeds, guava seeds, prickly pear seeds, calamansi seeds, pumpkin seeds, squash seeds, okra seeds, cucumber seeds, pepper seeds, eggplant seeds, pear seeds, apple seeds, cherimoya seeds, pineapple seeds, quince seeds, loquat seeds, nyger seeds, sugarcane seeds, or any other suitable seeds) may be ground to a particle size of about 5 to about 500 microns (e.g., about 5 to about 10 microns, about 10 to about 20 microns, about 20 to about 30 microns, about 25 microns, about 30 to about 50 microns, about 50 to about 100 microns, about 100 to about 150 microns, about 150 to about 200 microns, about 200 to about 300 microns, about 300 to about 400 microns, or about 400 to about 500 microns) and used as starting materials.The ground seeds are mixed for a suitable time (e.g., about 5 to about 120 minutes, about 10 to about 90 minutes, about 20 to about 60 minutes, about 30 to about 45 minutes, about 20 minutes, about 30 minutes, or about 40 minutes) while reaching a pH of about 5.5 to about 10.5 (e.g., about 5.5 to about 6.0, about 6.0 to about 6.5, about 6.5 to about 7.0, about 7.0 to about 7.4, about 7.4 to about 7.8, about 7.8 to about 8.2, about 8 to about 8.5, about 8.2 to about 8.6, about 8.6 to about 9, about 9 to about 9.5, about 9.5 to about 10.0, or about 10.0 to about 10.5), at a pressure of 0 to 10 bar (e.g., 0 to 2 bar, 2 to 4 bar, 4 to 6 bar, 6 to 8 bar, or 8 to 10 bar), and at a temperature of about 45°C to about 125°C (e.g., about 45°C to about 55°C, about 55°C to about 75°C, about 65°C to about 85°C, about 75°C to about 95°C, about 85°C to about 105°C, about 95°C to about 115°C, about 105°C to about 125°C, about 70°C, about 75°C, or about 80°C), with a caustic agent (e.g., sodium hydroxide, potassium hydroxide, sodium carbonate, calcium carbonate, calcium hydroxide, potassium hydrogen carbonate, hydrogen peroxide, or iodine) and water. The seed mixture can then be dried (e.g., by tray drying, spray drying, drum drying, falling film evaporation, freeze drying, or vacuum drying). The mixture is then combined with cocoa butter, an equivalent, substitute, or replacement of cocoa butter, and / or one or more other plant-derived oils, and then until reaching a final particle size of less than about 350 microns (e.g., about 300 to about 350 microns, about 250 to about 300 microns, about 200 to about 250 microns, about 150 to about 200 microns, about 125 to 150 microns, about 100 to about 125 microns, about 75 to about 100 microns, about 70 to about 75 microns, about 65 to about 70 microns, about 60 to about 65 microns, about 50 to about 60 microns, less than about 150 microns, less than about 100 microns, less than about 70 microns, less than about 65 microns, or less than about 60 microns), at a temperature of less than about 65°C (e.g., about 60°C to about 65°C, about 55°C to about 60°C, about 50°C to about 55°C, about 50°C to about 60°C, less than about 60°C, or less than about 55°C), and can be ground and / or purified (e.g., using a stone colander mill or a colloid mill).Next, the crushed mixture can be passed through a sieve (e.g., a 100 micron sieve) to obtain a bulking agent for inclusion in chocolate or another ingestible.
[0051] Any suitable method can be used to determine the particle size of the material produced from the milled seeds. In some cases, a micrometer screw gauge (micrometer caliper) or a Hegman gauge (also known as a grindometer) can be used. Other suitable methods include the use of a RoTap (rotary tap device) for dry materials, such as dry milled grape seeds or fruit seeds, a laser diffraction particle size analyzer, and a dynamic light scattering / laser diffraction analyzer.
[0052] For exemplary embodiments, particle size measurements were performed on dry and wet materials. For example, particle size measurements were performed on dry materials obtained from dry milling and grinding. Particle size measurements were also performed on wet materials obtained from wet milling and chocolate products.
[0053] Unless otherwise specified herein, when referring to the particle size of a dry material obtained from dry grinding or pulverization, the measurement was carried out using a RoTap. When referring to the particle size of a wet material, the measurement was carried out using a micrometer screw and / or a Hegman gauge. To monitor the particle size during the grinding process or to evaluate the chocolate product, often both a micrometer screw and a Hegman gauge are used. The particle size measurements of the control 60.1% standard Barry Callebaut chocolate, grape seed chocolate, a mixture of traditional chocolate and grape seed chocolate ("chocolate with extender"), cocoa-free chocolate, and other chocolate products of the present invention were carried out using a micrometer and / or a Hegman gauge. As described below, the particle sizes of the wet-milled grape seeds and the finished chocolate mass were also obtained by laser diffraction and / or dynamic light scattering / laser diffraction. An explanation of each method for testing the particle size of the materials of the present invention is provided below.
[0054] In some cases, complete plant seeds can be used as starting materials to prepare bulking agents. For example, complete seeds (e.g., grape seeds, cranberry seeds, raspberry seeds, blackberry seeds, strawberry seeds, blueberry seeds, pomegranate seeds, kiwi seeds, watermelon seeds, musk melon seeds, cantaloupe seeds, honeydew seeds, papaya seeds, passion fruit seeds, star fruit seeds, tomato seeds, cherry tomato seeds, dragon fruit seeds, guava seeds, prickly pear seeds, calamansi seeds, pumpkin seeds, squash seeds, okra seeds, cucumber seeds, pepper seeds, eggplant seeds, pear seeds, apple seeds, cherimoya seeds, pineapple seeds, quince seeds, amaranth (nyger) seeds, sesame seeds, or any other suitable seeds) can be sieved (e.g., using a mesh) to remove stem pieces and / or other unwanted plant materials. The sieved seeds can be treated with a caustic agent (e.g., sodium hydroxide, potassium hydroxide, sodium carbonate, calcium carbonate, calcium hydroxide, potassium hydrogen carbonate, hydrogen peroxide, or iodine) and water for an appropriate time (e.g., about 5 to about 120 minutes, about 10 to about 90 minutes, about 20 to about 60 minutes, about 30 to about 45 minutes, about 20 minutes, about 30 minutes, or about 40 minutes), while mixing, at a pressure of 0 to 10 bar (e.g., 0 to 2 bar, 2 to 4 bar, 4 to 6 bar, 6 to 8 bar, or 8 to 10 bar) and a temperature of about 55°C to about 95°C (e.g., about 55°C to about 75°C, about 65°C to about 85°C, about 75°C to about 95°C, about 70°C, about 75°C, or about 80°C) until a pH of about 5.5 to about 10 (e.g., about 5.5 to about 6.0, about 6.0 to about 6.5, about 6.5 to about 7.0, about 7.0 to about 7.4, about 7.4 to about 7.8, about 7.8 to about 8.2, about 8.2 to about 8.6, about 8.6 to about 9, about 9 to about 9.5, about 9.5 to about 10, or about 8 to about 8.5) is reached. Then, the seeds can be separated from the liquid by sieving to obtain a wet seed fraction and a liquid fraction containing dissolved solids. The wet seed fraction can be roasted (e.g., by air roasting, conduction roasting, direct fire roasting, or radiant heat roasting), and the liquid fraction can also be roasted (e.g., by dry roasting).Any suitable roasting temperature (e.g., from about 300°F to about 450°F, from about 325°F to about 425°F, or from about 350°F to about 400°F) can be used. The roasted wet seeds can then be milled (e.g., using a vermill, roller mill, pin mill, air classifier mill, hammer mill, colloid mill (when fat or liquid is added), stone mill, blade mill, jet mill, high impact mill, or espresso grinder) to achieve a particle size of from about 20 microns to about 300 microns (e.g., from about 20 to about 50 microns, from about 50 to about 75 microns, from about 75 to about 100 microns, from about 100 to about 150 microns, from about 150 to about 200 microns, from about 200 to about 250 microns, or from about 250 microns to about 300 microns). The roasted and milled wet seed fraction can then be recombined with the roasted liquid fraction. Cocoa butter or one or more vegetable oils (e.g., corn oil, sunflower oil, palm oil, coconut oil, shea oil, illipe oil, mango kernel oil, palm kernel oil, canola oil, avocado oil, safflower oil, or any other suitable vegetable oil) can be added and the mixture can be milled (e.g., using a stone colander mill or colloid mill) at a temperature of less than about 65°C (e.g., from about 60°C to about 65°C, from about 55°C to about 60°C, from about 50°C to about 55°C, from about 50°C to about 60°C, less than about 60°C, or less than about 55°C) until a final particle size of less than about 350 microns (e.g., from about 300 to about 350 microns, from about 250 to about 300 microns, from about 200 to about 250 microns, from about 150 to about 200 microns, from about 125 to 150 microns, from about 100 to about 125 microns, from about 75 to about 100 microns, from about 70 to about 75 microns, from about 65 to about 70 microns, from about 60 to about 65 microns, from about 50 to about 60 microns, less than about 150 microns, less than about 100 microns, less than about 70 microns, less than about 65 microns, or less than about 60 microns) is reached. The milled mixture can then be passed through a sieve (e.g., a 100 micron sieve) to obtain a bulking agent for inclusion in chocolate or other ingestibles.
[0055] Other methods of preparing an extender from whole plant seeds may include cleaning the whole seeds (e.g., using one or more of a destoner, a scalping deck, a suction channel, a sizing deck, an optical sorter, and a sieve) to remove unwanted husks, broken material, and other products of agricultural origin (e.g., stones, fruit peels, stems, branches, etc.). The whole seeds can be treated with a caustic solution (e.g., sodium hydroxide, potassium hydroxide, sodium carbonate, calcium carbonate, calcium hydroxide, potassium hydrogen carbonate, hydrogen peroxide, or iodine) and water at a suitable time (e.g., about 5 to about 120 minutes, about 10 to about 90 minutes, about 20 to about 60 minutes, about 30 to about 45 minutes, about 20 minutes, about 30 minutes, or about 40 minutes) while stirring, at a pressure of 0 to 10 bar (e.g., 0 to 2 bar, 2 to 4 bar, 4 to 6 bar, 6 to 8 bar, or 8 to 10 bar), and at an elevated temperature (e.g., about 55°C and about 95°C, about 55°C to about 75°C, about 65°C to about 85°C, about 75°C to about 95°C, about 70°C, about 75°C, or about 80°C) until a pH of about 7.8 to about 9.2 (e.g., about 7.8 to about 8.2, about 8.2 to about 8.6, about 8.6 to about 9, about 9 to about 9.2, or about 8 to about 9) is reached. In some cases, the treated seeds can be dewatered, in which case the seed mixture can be dried (e.g., by tray drying, spray drying, drum drying, or vacuum drying). The seeds can be screened to separate the wet seeds from the liquid, and the two streams can be dried separately. Alternatively, a vacuum can be applied to evaporate the moisture from the seed slurry. In some cases, one or more enzymes (e.g., cellulase, tannase, pectinase, xylanase, or hemicellulose) can optionally be added to the seeds together with water and / or one or more additional agents (e.g., a caustic material, an acidulant, or hydrogen peroxide). The seeds and solids can be roasted using, for example, convection, conduction, infrared, or a combination thereof.Next, the roasted seeds and other solids from the roasting step are ground using, for example, a crushing mill, a burr mill, an espresso grinder, a stone mill, a blade mill, a hammer mill, an air classification mill, a high impact mill, or a jet mill, and optionally sieved to obtain an extender for inclusion in chocolate or another ingestible.
[0056] This document also provides a method for manufacturing a composition (e.g., chocolate and other ingestibles) containing the extender provided herein. Any suitable method can be used to prepare a composition (e.g., chocolate or other ingestible) containing the extender provided herein. In some cases, the method may include combining the extender provided herein (e.g., grape seed extender) in any suitable amount with cocoa butter, sugar, and optionally cocoa solids. In some cases, the method may include combining the extender provided herein (e.g., grape seed extender) in any suitable amount with a substitute, replacement, or equivalent of cocoa butter (CBE), sugar, optionally cocoa solids, and optionally seed meal to produce a composition (e.g., chocolate and other ingestibles) that does not contain a cocoa component (e.g., a composition in which all of the cocoa solids and / or cocoa butter have been replaced with cocoa-free components). For example, the composition provided herein may contain from about 0.01 wt% to about 35 wt% (e.g., about 0.01 wt% to about 0.05 wt%, about 0.05 wt% to about 0.1 wt%, about 0.1 wt% to about 0.5 wt%, about 0.5 wt% to about 1 wt%, about 1 wt% to about 5 wt%, about 5 wt% to about 10 wt%, about 10 wt% to about 15 wt%, about 15 wt% to about 20 wt%, about 20 wt% to about 25 wt%, about 25 wt% to about 30 wt%, about 30 wt% to about 35 wt%, about 10 wt%, about 12.5 wt%, about 15 wt%, about 17.5 wt%, about 20 wt%, about 22.5 wt%, or about 25 wt%) of an extender (e.g., grape seed extender).
[0057] In some cases, the compositions provided herein may contain from about 20 wt% to about 55 wt% (e.g., from about 20 wt% to about 25 wt%, from about 25 wt% to about 30 wt%, from about 30 wt% to about 35 wt%, from about 35 wt% to about 40 wt%, from about 40 wt% to about 45 wt%, from about 45 wt% to about 50 wt%, from about 50 wt% to about 55 wt%, about 30 wt%, about 32.5 wt%, about 35 wt%, about 37.5 wt%, about 40 wt%, about 42.5 wt%, or about 45 wt%) of cocoa butter.
[0058] In some cases, the compositions provided herein may contain from about 20 wt% to about 60 wt% (e.g., from about 20 wt% to about 25 wt%, from about 25 wt% to about 30 wt%, from about 30 wt% to about 35 wt%, from about 35 wt% to about 40 wt%, from about 40 wt% to about 45 wt%, from about 45 wt% to about 50 wt%, from about 50 wt% to about 55 wt%, from about 55 wt% to about 60 wt%, about 35 wt%, about 37.5 wt%, about 40 wt%, about 42.5 wt%, or about 45 wt%) of sugar (e.g., sucrose, glucose, lactose, fructose, or maltose).
[0059] In some cases, the compositions provided herein may contain from about 0.5 wt% to about 25 wt% (e.g., from about 0.5 wt% to about 0.75 wt%, from about 0.75 wt% to about 1 wt%, from about 1 wt% to about 3 wt%, from about 3 wt% to about 4 wt%, from about 4 wt% to about 5 wt%, from about 5 wt% to about 5.5 wt%, from about 5.5 wt% to about 6 wt%, from about 6 wt% to about 7 wt%, from about 7 wt% to about 10 wt%, from about 10 wt% to about 15 wt%, from about 15 wt% to about 20 wt%, from about 20 wt% to about 25 wt%, about 4.5 wt%, about 5 wt%, about 5.5 wt%, about 6 wt%, or about 6.5 wt%) of cocoa solids.
[0060] In some cases, chocolate can be prepared from cocoa butter (and / or CBE), sugar, optionally cocoa solids, optionally seed meal, and / or optionally lecithin, combined with the bulking agent provided herein. For example, a bulking agent (e.g., grape seed bulking agent) can be combined with cocoa butter (or CBE), sugar, and optionally cocoa solids and / or seed meal and mixed with grinding for 24 to 72 hours (e.g., 24 to 36, 36 to 48, 48 to 60, or 60 to 72 hours) to obtain a particle size of about 25 to 35 microns. The resulting chocolate can be tempered, molded, subsequently cooled, and removed from the mold.
[0061] In some cases, a bulking agent (e.g., grape seed bulking agent) can be mixed with one or more sugars, cocoa butter (and / or CBE), and optionally cocoa solids and / or oil seed meal (e.g., at about 30 to about 40 °C for about 10 to about 60 minutes). The combination can be emulsified at a suitable temperature (e.g., using a ball mill) until the particle size is less than about 30 microns (e.g., less than 25 microns or less than 20 microns). The resulting chocolate can then be solidified (e.g., at about 10 to about 15 °C in a mold block). In some cases, the chocolate can be removed from the mold and optionally further processed. For example, the chocolate can be melted, tempered, deposited in a mold (e.g., a bar mold), cooled (e.g., at about 5 °C to about 20 °C, or about 10 °C to about 15 °C), or deposited on a cooling belt to make chips or chunks.
[0062] In some cases, a bulking agent (e.g., grape seed bulking agent) can be mixed with one or more sugars, cocoa butter (and / or CBE), and optionally cocoa solids and / or oilseed meal (e.g., at about 30 °C to about 40 °C, or at about 35 °C) to homogenize the mixture. The resulting slurry can be pumped to a particle size reduction machine (e.g., a continuous rotor stator particle size reduction machine) by any suitable means (e.g., medium / high tip speed with a corrugated barrel). The material can optionally be homogenized and additional components (if present) can be added. Then, the mixture can be pumped to a refiner to reduce the particle size of the material to less than about 30 microns (e.g., less than about 25 microns or less than about 20 microns). Then, the material can be conveyed to a liquefier or conche to create the final texture. The chocolate can optionally be tempered and then solidified at a temperature of about 5 °C to about 20 °C (e.g., about 10 °C to about 15 °C), for example, in a mold or on a belt slab. Then, the chocolate can be removed from the mold and optionally packaged or wrapped (e.g., for further processing or for use as an industrial ingredient). For further processing, the chocolate can be melted at a high temperature (e.g., higher than about 25 °C, higher than about 30 °C, or higher than about 35 °C). The melted chocolate can be tempered to obtain the desired fat crystal structure and then placed in a mold (e.g., a bar mold) and cooled (e.g., at about 5 °C to about 20 °C, or about 10 °C to about 15 °C), or deposited on a cooling belt to make chips or chunks.
[0063] In some cases, a bulking agent (e.g., grape seed bulking agent) can be mixed with one or more sugars, cocoa butter (and / or CBE), and optionally cocoa solids and / or seed meal (e.g., at about 30°C to about 40°C, or at about 35°C) to homogenize the mixture. The resulting slurry can be pumped, for example, to a 2-roll prefinisher and then to a homogenizing screw to homogenize the material with additional ingredients (if present). The mixture can be transported directly to a refiner to reduce the particle size of the material to less than about 30 microns (e.g., less than about 25 microns or less than about 20 microns). The material can be transported to a liquefier or conche to create the final texture. In some cases, the material can be pumped to a ball mill (e.g., a continuous ball mill) to further reduce the particle size. The resulting chocolate can optionally be tempered and then solidified at a temperature of about 5°C to about 20°C (e.g., about 10°C to about 15°C), for example, in a mold or on a belt slab. The chocolate can then be removed from the mold and optionally packaged or wrapped (e.g., for further processing or use as an industrial ingredient). For further processing, the chocolate can be melted at a high temperature (e.g., higher than about 25°C, higher than about 30°C, or higher than about 35°C). The melted chocolate can be tempered to obtain the desired fat crystal structure and then placed in a mold (e.g., a bar mold) and cooled (e.g., at about 5°C to about 20°C, or at about 10°C to about 15°C), or deposited on a cooling belt to make chips or chunks.
[0064] In some cases, the methods provided herein can be used to produce chocolate beans. For example, a bulking agent having a particle size of about 20 to about 150 μm can be combined with cocoa butter, sugar, and optionally cocoa solids (e.g., by the mixing and additional processes as described above). In some cases, a tableting aid (e.g., one or more cereal or non-cereal components such as binders like starch, sugar, and / or gum that can assist in tableting) can be added. The mixture can then be tableted (e.g., with a pill press or similar device) so that chocolate beans are formed. Optionally, the chocolate beans can be coated, for example, with shellac, zein protein, or wax.
[0065] In any method for manufacturing the compositions provided herein, it should be noted that chocolate containing a bulking agent (e.g., grape seed bulking agent or berry seed bulking agent), cocoa butter (or CBE), and sugar can be produced and then optionally combined with "traditional" chocolate containing cocoa butter, sugar, and cocoa solids. In such methods, a portion of the cocoa solids of the traditional chocolate (e.g., about 0.1 wt% to about 75 wt%, e.g., about 0.1 wt% to about 0.5 wt%, about 0.5 wt% to about 1 wt%, about 1 wt% to about 3 wt%, about 3 wt% to about 5 wt%, about 5 wt% to about 10 wt%, about 10 wt% to about 15 wt%, about 15 wt% to about 20 wt%, about 20 wt% to about 25 wt%, about 25 wt% to about 30 wt%, about 30 wt% to about 40 wt%, about 40 wt% to about 50 wt%, about 50 wt% to about 60 wt%, or about 60 wt% to about 75 wt%) can be replaced with the bulking agent.
[0066] In some cases, the chocolate formulation can include, in suitable proportions, the extenders provided herein, one or more sugars, and one or more fats (e.g., cocoa butter and / or alternatives, substitutes, or equivalents for cocoa butter, and / or optionally oilseed meal and / or lecithin). In some cases, the chocolate formulation can include, for example, a suitable proportion of oilseed meal (e.g., sunflower meal) when using a higher proportion of extender product. In some cases, the chocolate formulation can include from 0 to 30 wt% of seed meal, from 0 to 20 wt% of seed meal, or from 7 to 20 wt% of seed meal. In some cases, the chocolate formulation can include 10 - 20 wt% of extender, 30 - 55 wt% of sugar, 25 - 45 wt% of cocoa butter substitute, 7 - 20 wt% of seed meal, and 0.25 - 0.75 wt% of lecithin.
[0067] Generally, oilseed meals, also known as seed meals, are by-products from the production of oils for human consumption. This group includes rapeseed meal, canola meal, cottonseed meal, flaxseed meal, sunflower meal, and camelina (wild flax) meal. In some cases, some or all of the cocoa butter in the composition can be replaced with one or more cocoa butter alternatives, substitutes, and / or equivalents (CBEs). Cocoa butter alternatives, substitutes, and equivalents include, for example, other vegetable fat raw materials and hardstock fats (fats that are solid at room temperature). Examples of such vegetable fat raw materials and hardstock fats include, but are not limited to, shea, illipe, palm oil, Shorea robusta, kokum gurgi (Garcinia indica), mango kernel (Mangifera indica), coconut, oil blends, fractionated oils, and / or interesterified oils. In some cases, vegetable fats can include a blend of two or more hardstock fats (e.g., a 50%:50% blend of palm oil:shea oil). In some cases, vegetable fats can include one or more cocoa butter equivalents blended with cocoa butter (e.g., a 75%:25% blend of palm oil:cocoa butter) to provide some of the flavor and aroma characteristics of pure cocoa butter without the expense. In some cases, vegetable fats can include one or more hardstock fats blended with one or more liquid vegetable oils (e.g., a 75%:25% blend of palm oil:rapeseed oil) to create a blended fat. In some cases, a blend of a hardstock fat and an oil that is liquid at room temperature can provide a blended product having some of the desired characteristics of the pure hardstock fat.
[0068] In some embodiments, the complete seeds described herein are cleaned with machines such as destoners, scalping decks, aspiration channels, sizing decks, optical sorters, sieves, or combinations thereof. For example, a destoner can separate particles based on density and remove heavier impurities such as rocks and glass; a scalping deck can separate particles by size and remove larger impurities such as large branches; an aspiration channel can be used to blow air to further clean materials such as stems that cannot be completely removed by other machines (e.g., destoners and scalping decks); a sizing deck is similar to a scalping deck but can use smaller or larger screens to obtain only materials of a desired size; a sieve is also similar but is often used to remove husks or dust; an optical sorter that uses highly sophisticated optical imaging to target impurities that can be removed from the product by compressed air can be used for combinations of the above purposes.
[0069] In some embodiments, the complete seeds described herein are treated chemically and / or enzymatically (e.g., by a chemical solution or a solution containing an enzyme), either simultaneously or sequentially. Non-limitingly, the complete seeds can be treated with a chemical solution containing a caustic agent, an acidulant, or an oxidizing agent such as hydrogen peroxide. Acidulants can include, non-limitingly, acetic acid, adipic acid, citric acid, fumaric acid, lactic acid, malic acid, phosphoric acid, and tartaric acid, and / or glucono-delta-lactone. The complete seeds can be treated enzymatically with one or more of the foregoing enzymes (e.g., cellulase, tannase, pectinase, xylase, or hemicellulose). When the treatment includes a chemical method with a caustic solution, the caustic agent can be, for example, sodium hydroxide, potassium hydroxide, sodium carbonate, calcium carbonate, calcium hydroxide, potassium bicarbonate, or iodine, which can be applied to the complete seeds at ambient or elevated temperature and / or at atmospheric or supra-atmospheric pressure. The treatment can be carried out by various methods including immersion, spraying, boiling, stirring, coating, or combinations of these methods to expose the complete seeds and / or their husks to chemical and / or enzymatic agents. In some embodiments, the complete seeds are treated with a chemical and / or enzymatic agent in an aqueous solution at elevated temperature (e.g., 75°C to 100°C) for 30 minutes to 2 hours while stirring to reach a pH of 8 to 10.
[0070] In some embodiments, non-limiting examples include grinding by one or more dry grinding techniques and / or one or more wet grinding techniques, including but not limited to the use of a wet grinder, a crushing mill, a bar mill, an espresso grinder, a stone mill, a jet mill, a bar mill, a roller mill, a pin mill, an air classification mill, a hammer mill, a colloid mill (when fat or liquid is added to the dry material), a corundum mill, a stone mill, a blade mill, or a high impact mill, to grind the seeds and / or solids described herein. Dry grinding is used to grind dry materials with little or no oil and / or moisture and is also useful for coarse grinding into pieces or larger particles. Dry grinding can also be used to reduce the particle size to about 100 μm.
[0071] Wet grinding (wet milling technology) can be used to reduce particle size and can grind materials (e.g., roasted grape seeds or roasted fruit seeds) to a refined paste that, in some cases, is less than 100 μm, in some cases less than about 40 μm, in some cases less than 35 μm, or in some cases about 25 μm. Examples of grinders for wet grinding include, without limitation, colloid mills, corundum mills, stone mills, and blade mills. Wet grinding can be carried out by adding a liquid medium such as water or liquid oil so as to act as a lubricant during the grinding process. Depending on whether the final product is a water-based product or a fat-based product, either water or fat / oil can be added for wet grinding. To produce the fat-based chocolate product of the present invention, in order to enable a finer particle size, fat or liquid oil (e.g., cocoa butter or cocoa butter equivalents) can be added to the seeds before grinding and then grinding can be carried out in the fat. Some advantages of wet grinding include a reduced explosion risk at finer final particle sizes, lower capital investment, and ease of grinding effectiveness for a wider range of materials, particularly when the material to be ground, such as grape seeds, contains endogenous oil (i.e., grape seed oil). Wet grinding is a particularly effective technique for grinding oil-containing seeds such as grape seeds and fruit seeds after roasting to produce extenders having a reduced particle size. In some embodiments, to produce wet-ground grape seeds or fruit seeds for the extenders and compositions of the present invention, 30-60 wt% of fat or liquid oil is added to the roasted grape seeds and wet grinding is carried out in a fat / oil medium by grinding, for example, in a stone mill (e.g., stone melanger), colloid mill, blade mill, or corundum mill.
[0072] Exemplary embodiments Embodiment 1 is a composition consisting essentially of roasted and ground fruit seeds wherein the ground fruit seeds have a particle size of less than 350 microns.
[0073] Aspect 2 is the composition of Aspect 1, wherein the fruit seed is a grape seed.
[0074] Aspect 3 is the composition of Aspect 2, wherein the grape seed is from edible grapes, Concord, Niagara, Chardonnay, Sauvignon Blanc, Muscat, Sultana, Riesling, Pinot Gris, Pinot Grigio, Cabernet Sauvignon, Merlot, Pinot Noir, Shiraz, Albariño, Malbec, Grüner Veltliner, Solaris, Zinfandel, Cabernet Franc, Tempranillo, Carmenère, Mataro, Sangiovese, Regent, Black Muscat, Chasselas, Wild Grape, Nebbiolo, Montepulciano, Gewürztraminer, Barbera, Schönburger, Carignan, Semillon, Gamay, Petit Verdot, Trebbiano, Sancerre, Grüner Veltliner, Silvaner, Petit Syrah, or Grüner Veltliner Blanc.
[0075] Aspect 4 is the composition of Aspect 1, wherein the fruit seed is derived from cranberry, raspberry, blueberry, strawberry, blackberry, pomegranate, kiwi, watermelon, muskmelon, cantaloupe, honeydew, papaya, passion fruit, star fruit, tomato, tomatillo, dragon fruit, guava, prickly pear, calamansi, pumpkin, squash, okra, cucumber, bell pepper, eggplant, pear, apple, cherimoya, pineapple, quince, loquat, date palm, or fenugreek.
[0076] Aspect 5 is the composition of any one of Aspects 1 to 4, wherein the ground fruit seed has a particle size of less than 250 microns.
[0077] Aspect 6 is the composition of any one of Aspects 1 to 4, wherein the ground fruit seed has a particle size of less than 150 microns.
[0078] Aspect 7 is an ingestible product comprising a bulking agent consisting essentially of roasted and ground fruit seeds, wherein the ground fruit seeds have a particle size of less than 350 microns.
[0079] Aspect 8 is an ingestible product of Aspect 7 that is chocolate.
[0080] Aspect 9 is an ingestible product of Aspect 8, wherein the chocolate contains about 0.01 wt% to about 35 wt% of a bulking agent; about 20 wt% to about 55 wt% of cocoa butter; about 20 wt% to about 60 wt% of sugar; and optionally about 0.5 wt% to about 25 wt% of cocoa solids.
[0081] Aspect 10 is an ingestible product of Aspect 8, wherein the chocolate contains about 17.5 wt% of a bulking agent; about 37.5 wt% of cocoa butter; about 40 wt% of sugar; and optionally about 5 wt% of cocoa solids.
[0082] Aspect 11 is an ingestible product of any one of Aspects 7 to 10, wherein the fruit seed is a grape seed.
[0083] Aspect 12 is an ingestible product of Aspect 11, wherein the grape seed is derived from grapes of edible grapes, Concord, Niagara, Chardonnay, Sauvignon Blanc, Muscat, Sultana, Riesling, Pinot Gris, Pinot Grigio, Cabernet Sauvignon, Merlot, Pinot Noir, Shiraz, Albariño, Malbec, Grüner Veltliner, Solaris, Zinfandel, Cabernet Franc, Tempranillo, Carmenère, Mataro, Sangiovese, Regent, Black Muscat, Chasselas, Wild Grape, Nebbiolo, Montepulciano, Gewürztraminer, Barbera, Schönburger, Carignan, Semillon, Gamay, Petit Verdot, Trebbiano, Sancerre, Grüner Veltliner, Silvaner, Petit Syrah, or Grüner Veltliner Blanc.
[0084] Aspect 13 is an ingestible product of any one of Aspects 7-10, wherein the fruit seeds are derived from cranberry, raspberry, blueberry, strawberry, blackberry, pomegranate, kiwi, watermelon, muskmelon, cantaloupe, honeydew, papaya, passion fruit, star fruit, tomato, cherry tomato, dragon fruit, guava, prickly pear, calamansi, pumpkin, squash, okra, cucumber, pepper, eggplant, pear, apple, cherimoya, pineapple, quince, loquat, date palm, or fenugreek.
[0085] Aspect 14 is an ingestible product of any one of Aspects 7-13, wherein the ground fruit seeds have a particle size of less than 250 microns.
[0086] Aspect 15 is an ingestible product of any one of Aspects 7-13, wherein the ground fruit seeds have a particle size of less than 150 microns.
[0087] The present invention will be further described in the following examples, which are not intended to limit the scope of the invention described in the claims.
Examples
[0088] Example 1 - Processing of Seed Material (at Changing pH as a Solution) The seed material was processed according to the following procedure.
[0089] 1. To remove husks, broken materials, and other products of agricultural origin (e.g., stones, skins, stems, and branches), the complete seeds were washed with machines such as destoners, scalping decks, suction channels, sizing decks, optical sorters, sieves, or combinations thereof. The target impurities at the end of the washing process were less than 0.5% w / w. To determine the impurities, a 1-kilogram sample of the washed complete seeds was visually inspected and hand-sorted to remove husks, broken materials, and other products that were not removed during the washing process. This yielded two hand-sorted samples, which were weighed. The impurities were reported as a percentage of the washed sample.
[0090] 2. The complete seeds were treated with a caustic solution in water (e.g., sodium hydroxide, potassium hydroxide, sodium carbonate, calcium carbonate, calcium hydroxide, potassium hydrogen carbonate, hydrogen peroxide, or iodine) at a high temperature (e.g., 75°C to 100°C) for 30 minutes to 2 hours while stirring to reach a pH of 8 to 10. It was observed that the increase in pH was a function of both the temperature and the length of time when stirring the seeds in the caustic solution; treatment of the complete seeds in the caustic solution at the upper limit of the temperature range of 75°C to 100°C and / or at the upper limit of the time length range of 30 minutes to 2 hours resulted in a pH at the upper limit of the range of 8 to 10. In some examples, the complete seeds were treated enzymatically with a solution containing an enzyme (e.g., cellulase and / or hemicellulase) in an aqueous solution for 30 minutes to 2 hours while stirring, either with, before, or after treatment with the caustic solution. The enzyme was observed to assist in the breakdown of the tough and lignan-rich fibrous material of grape seeds or fruit seeds.
[0091] 3. The seeds were sieved, and the two resulting streams were dried separately and / or the liquid was aspirated and removed using vacuum to evaporate the moisture from the slurry. The target moisture content after drying was 2 - 10% w / w, preferably 6% w / w. When vacuum was applied to the slurry itself, the target moisture content was less than 25% w / w (preferably 20% w / w). Based on the loss-on-drying method, a moisture meter was used to measure the moisture content. The wet sample was weighed on a scale, placed in an oven, and heated until the end of the drying period, i.e., until the sample reached equilibrium. The weight loss was the moisture content of the sample.
[0092] 4. The seeds and solids from step 3 were roasted at 140 - 200 °C, preferably 150 - 175 °C, using convection, conduction, or a combination of the two for about 20 minutes to 2 hours (e.g., about 45 minutes). After roasting was complete, the seeds were observed to have changed color to a dark brown and to have produced coffee-like sensory notes. When seeds with a pH adjusted to the upper limit in the range of 8 - 10 in step 2 were roasted, the dark brown color was particularly prominent. The target moisture content after roasting was less than 2% w / w. Based on the loss-on-drying method, a moisture meter was used to measure the moisture content. The wet sample was weighed on a scale, placed in an oven, and heated until the end of the drying period, i.e., until the sample reached equilibrium. The weight loss was the moisture content of the sample.
[0093] 5. Seeds and other solids from the roasting process were ground using a grinder (e.g., a wet grinder, a crushing mill, a bar mill, an espresso grinder, a stone mill, or a jet mill) into a refined paste having a particle size of 350 μm or less (preferably 150 μm or less), and optionally sieved to remove unwanted materials. For example, after grinding in the grinder, sieving with a sieve or mesh made it possible to remove larger particles or foreign matter (e.g., leaves or stems) that had passed through the previous seed material processing steps by mistake. For some examples of wet grinding, a fat or liquid oil (e.g., a vegetable fat such as cocoa butter or a cocoa butter equivalent) was added to the seeds before grinding and then ground into a paste. A fat in an amount of 30 - 60% by weight was added to the roasted grape seeds and wet ground to produce a paste-like wet ground grape seed. The wet grinding was carried out with a stone mill (e.g., a stone melanger), a colloid mill, a blade mill, or a corundum mill.
[0094] Example 2 - Processing of Seed Material (at Changing pH as a Dispersion) The seed material was processed according to the following procedure.
[0095] 1. The whole seeds were cleaned using machines such as a destoner, a scalping deck, a suction channel, a sizing deck, an optical sorter, a sieve, or a combination thereof to remove the husks, broken materials, and other products of agricultural origin (e.g., stones, skins, stems, and branches). The target impurities at the end of the cleaning process were less than 0.5% w / w. To measure the impurities, a 1 - kilogram sample of the cleaned whole seeds was visually inspected and hand - sorted to remove the husks, broken materials, and other products that were not removed during the cleaning process. This yielded two hand - sorted samples, which were weighed. The impurities were reported as a percentage of the cleaned sample.
[0096] 2. While stirring, at a high temperature (e.g., 60 °C to 125 °C), spray a caustic solution (e.g., sodium hydroxide, potassium hydroxide, sodium carbonate, calcium carbonate, calcium hydroxide, potassium hydrogen carbonate, hydrogen peroxide, or iodine) onto the complete seeds, mix until a pH of 5.5 to 10.5 is reached, disperse and coat each seed. It was observed that the increase in pH is a function of both the temperature and the length of time when stirring the seeds with the caustic solution; treatment of the complete seeds with the caustic solution at the upper limit of the temperature in the range of 60 °C to 125 °C and / or at the upper limit of the length of time in the range of 30 minutes to 2 hours resulted in a pH at the upper limit of the range of 5.5 to 10.5. In some examples, with or before or after treatment with the caustic solution, the complete seeds were enzymatically treated with a solution containing an enzyme (e.g., cellulase and / or hemicellulase) in an aqueous solution while stirring for 30 minutes to 2 hours. The enzyme was observed to assist in the breakdown of the tough and lignan-rich fibrous material of grape seeds or fruit seeds. Optionally, under vacuum, the temperature was raised to evaporate water and dry the seeds. The target moisture content at the end of this step was less than 25% w / w moisture. Based on the drying loss method, a moisture meter was used to measure the moisture content. The wet sample was weighed on a scale, placed in an oven, and heated until the end of the drying period, i.e., until the sample reached equilibrium. The weight loss is the moisture content of the sample.
[0097] 3. Roast the seeds at 140 to 200 °C, preferably 150 to 175 °C, using convection, conduction, or a combination of the two. The target moisture content was less than 2% w / w. Based on the drying loss method, a moisture meter was used to measure the moisture content. The wet sample was weighed on a scale, placed in an oven, and heated until the end of the drying period, i.e., until the sample reached equilibrium. The weight loss is the moisture content of the sample. For example, the dried seeds were roasted in a convection roaster at a temperature of 140 °C to 200 °C for 20 minutes to 2 hours to obtain roasted seeds. After roasting was complete, the seeds were observed to turn dark brown and produce coffee-like sensory notes. When roasting seeds whose pH was adjusted to the upper limit of the pH range in step 2, the dark brown color was particularly prominent.
[0098] 4. Seeds and other solids from the roasting process are ground using a grinder (e.g., a wet grinder, a crushing mill, a bar mill, an espresso grinder, a stone mill, or a jet mill) into a refined paste having a particle size of 350 μm or less (preferably 150 μm or less), and optionally sieved to remove unwanted materials. For example, after grinding in the grinder, it was possible to remove larger particles or foreign matter (e.g., leaves or stems) that had passed through the previous seed material processing steps by sieving with a sieve or mesh. For wet grinding used to further purify the product, a fat or liquid oil (e.g., a vegetable fat such as cocoa butter or a cocoa butter equivalent) was added to the seeds before grinding and then ground into a paste. A fat in an amount of 30 - 60% by weight was added to the roasted grape seeds and wet ground in the fat to produce a paste-like wet ground grape seed. The wet grinding was carried out using a stone mill (e.g., a stone melanger), a colloid mill, a blade mill, or a corundum mill.
[0099] Example 3 - Processing of Seed Material (at Changing pH in a Reaction Vessel) The seed material was processed according to the following procedure.
[0100] 1. The whole seeds were cleaned using machines such as a destoner, a scalping deck, a suction channel, a sizing deck, an optical sorter, a sieve, or a combination thereof to remove the husks, broken materials, and other products of agricultural origin (e.g., stones, skins, stems, and branches). The target impurities at the end of the cleaning process were less than 0.5% w / w. To measure the impurities, a 1 - kilogram sample of the cleaned whole seeds was visually inspected and hand - sorted to remove the husks, broken materials, and other products that were not removed during the cleaning process. This resulted in two samples that were hand - sorted and weighed. The impurities were reported as a percentage of the cleaned sample.
[0101] 2. While stirring at the bottom of the reaction chamber, until a pH of 5.5 to 10.5 is reached, a solution containing just enough water to fluidize the seeds is used, and a caustic solution (e.g., sodium hydroxide, potassium hydroxide, sodium carbonate, calcium carbonate, calcium hydroxide, potassium hydrogen carbonate, hydrogen peroxide, or iodine) is applied to the intact seeds. It has been observed that the increase in pH is a function of both the temperature and the length of time during which the seeds are stirred in the caustic solution; treatment of the intact seeds in the caustic solution at the upper limit of the temperature range of 75 °C to 100 °C and / or at the upper limit of the length of time range of 30 minutes to 2 hours resulted in a pH at the upper limit of the range of 5.5 to 10.5. In some examples, along with, before, or after treatment with the caustic solution, the intact seeds were enzymatically treated for 30 minutes to 2 hours while stirring with a solution containing an enzyme (e.g., cellulase and / or hemicellulase) in an aqueous solution. The enzyme was observed to assist in the breakdown of the tough and lignan-rich fibrous material of the intact seeds.
[0102] 3. The material was heated at a pressure 1 to 3 bar higher than atmospheric pressure for 10 minutes to 2 hours, and steam and / or pressure were used to accelerate the pH adjustment process. The application of high-pressure steam (or non-high-pressure steam), when used, decreased the amount of time required to change the observed pH of the intact seed reaction mixture and the treated seeds to 5.5 to 10.5. In any variation of this step, the pH adjustment process was carried out using steam without applying a pressure higher than atmospheric pressure. In another optional variation of this step, the pH adjustment process was carried out at atmospheric pressure without adding steam. All three variations of this step resulted in treated seeds with a pH of 5.5 to 10.5 being observed.
[0103] 4. Once the pH adjustment step was completed, optionally, the solution was aspirated using vacuum suction (drawing) to partially dry the seeds. The application of vacuum suction reduced the water content, and the water content at the end of this step was less than 25% w / w moisture and less than 20% w / w moisture. The target water content at the end of this step is less than 25% w / w moisture, preferably less than 20% w / w moisture. Based on the loss-on-drying method, a moisture meter was used to measure the water content. The wet sample was weighed on a scale, placed in an oven, and heated until the end of the drying period, i.e., until the sample reached equilibrium. The weight loss is the water content of the sample. When not using vacuum suction, the wet seeds were partially dried by the application of a weak heat at a slightly elevated temperature of 120 - 160°F.
[0104] 5. The seeds were roasted at 140 - 200°C, preferably 150 - 175°C, using convection, conduction, or a combination of the two. The target water content after roasting was less than 2% w / w.
[0105] 6. The roasted seeds and other solids from the roasting step were ground into a refined paste having a particle size of 350 μm or less (preferably 150 μm or less) using a grinder (e.g., a wet grinder, a crushing mill, a burr mill, an espresso grinder, a stone mill, or a jet mill), and optionally sieved to remove unwanted materials. For wet grinding, a fat or liquid oil (e.g., a vegetable fat such as cocoa butter or a cocoa butter equivalent) was added to the seeds before grinding and then ground into a paste. A fat in an amount of 30 - 60% by weight was added to the roasted grape seeds and wet ground in the fat to produce a pasty wet ground grape seed. The wet grinding was carried out using a stone mill (e.g., a stone melanger), a colloid mill, a blade mill, or a corundum mill.
[0106] Example 4 - Processing of Seed Material (at Changing pH in a Roaster) The seed material was processed according to the following procedure.
[0107] 1. The complete seeds were washed with machinery such as destoners, scalping decks, suction channels, sizing decks, optical sorters, sieves, or combinations thereof to remove husks, broken materials, and other agricultural-origin products (e.g., stones, skins, stems, and branches). The target impurities at the end of the washing process were less than 0.5 w / w%. To measure the impurities, a 1-kilogram sample of the washed complete seeds was visually inspected and hand-sorted to remove husks, broken materials, and other products that were not removed during the washing process. This yielded two hand-sorted samples, which were weighed. The impurities were reported as a percentage of the washed sample.
[0108] 2. While stirring, a caustic solution (e.g., sodium hydroxide, potassium hydroxide, sodium carbonate, calcium carbonate, calcium hydroxide, potassium hydrogen carbonate, hydrogen peroxide, or iodine) was sprayed onto the complete seeds at a high temperature (e.g., 60 °C to 125 °C), mixed until a pH of 5.5 to 10.5 was reached, and each seed was dispersed and coated. It was observed that the increase in pH was a function of both the temperature and the length of time when stirring the seeds with the caustic solution; treatment of the complete seeds with the caustic solution at the upper limit of the temperature range of 60 °C to 125 °C and / or at the upper limit of the time length range of 30 minutes to 2 hours resulted in a pH at the upper limit of the range of 5.5 to 10.5. In some examples, with or before or after treatment with the caustic solution, the complete seeds were treated enzymatically with a solution containing an enzyme (e.g., cellulase and / or hemicellulase) in an aqueous solution while stirring for 30 minutes to 2 hours. The enzyme was observed to assist in the decomposition of the tough and lignan-rich fibrous material of grape seeds or fruit seeds. The temperature and air speed were increased to evaporate the water and dry the seeds.
[0109] 3. The seeds were placed in a convection / conduction roaster.
[0110] 4. Once the seeds were dried, the roasting temperature was raised above 125 °C (e.g., up to 200 °C). The seeds were roasted using convection, conduction, or a combination of the two. For example, the dried seeds were roasted in a convection roaster at a temperature of 140 °C to 200 °C for 20 minutes to 2 hours to obtain roasted seeds. After roasting was completed, it was observed that the seeds had turned dark brown and produced coffee-like sensory notes. When the seeds with the pH adjusted to the upper limit of the pH range in Step 2 were roasted, the dark brown color was particularly prominent.
[0111] 5. The seeds and other solids from the roasting step were ground using a grinder (e.g., a wet grinder, a crushing mill, a burr mill, an espresso grinder, a stone mill, or a jet mill) into a refined paste having a particle size of 350 μm or less (preferably 150 μm or less), and optionally sieved to remove unwanted materials. For some examples of wet grinding, a fat or liquid oil (e.g., a vegetable fat such as cocoa butter or a cocoa butter equivalent) was added to the seeds before grinding and then ground into a paste. A fat in an amount of 30 to 60% by weight was added to the roasted grape seeds and wet ground in the fat to produce a pasty wet-ground grape seed. The wet grinding was carried out using a stone mill (e.g., a stone melanger), a colloid mill, a blade mill, or a corundum mill.
[0112] Example 5 - Processing of Seed Materials (Reagents during Dutching / Roasting) The seed materials were processed according to the following procedure.
[0113] 1. The complete seeds were cleaned using machinery such as a destoner, scalping deck, suction channel, sizing deck, optical sorter, sieve, or combinations thereof to remove husks, broken material, and other agricultural-origin products (e.g., stones, skins, stems, and branches). The target impurities at the end of the cleaning process were less than 0.5% w / w. To measure the impurities, a 1-kilogram sample of the cleaned complete seeds was visually inspected and hand-sorted to remove husks, broken material, and other products that were not removed during the cleaning process. This resulted in two hand-sorted samples, which were weighed. The impurities were reported as a percentage of the cleaned sample.
[0114] 2. While stirring, a caustic solution (e.g., sodium hydroxide, potassium hydroxide, sodium carbonate, calcium carbonate, calcium hydroxide, potassium bicarbonate, hydrogen peroxide, or iodine) containing any reaction components (e.g., sugars, amino acids, transition / catalyst metals, and / or salts) was sprayed onto the seeds at a high temperature (e.g., 60 °C to 150 °C), mixed until a pH of 5.5 to 10.5 was reached, and each seed was dispersed and coated. For example, the seeds were dutched to pH 8.5 with the solution. It was observed that the increase in pH was a function of both the temperature and the length of time during which the seeds were stirred with the caustic solution; treatment of the complete seeds in the caustic solution at the upper limit of the temperature range of 60 °C to 150 °C and / or at the upper limit of the time length range of 30 minutes to 2 hours resulted in the upper limit of the pH range of 5.5 to 10.5. In some examples, the complete seeds were treated enzymatically with a solution containing enzymes (e.g., cellulase and / or hemicellulase) in an aqueous solution for 30 minutes to 2 hours while stirring, either with, before, or after treatment with the caustic solution. The enzymes were observed to assist in the breakdown of the tough and lignan-rich fibrous material of the grape seeds. The temperature and air speed were increased to evaporate the water and dry the seeds.
[0115] 3. The seeds were placed in a convection / conduction roaster.
[0116] 4. Once dried, the roasting temperature was raised above 125°C (e.g., up to 200°C), and the seeds were roasted using convection, conduction, or a combination of the two. For example, the dried seeds were roasted in a convective roaster at a temperature of 140°C to 200°C for 20 minutes to 2 hours, e.g., for 30 minutes at 380°F, to obtain roasted seeds. After roasting was complete, the seeds were observed to have changed color to a dark brown and to have developed coffee-like sensory notes. When seeds with the pH adjusted to the upper limit of the pH range in Step 2 were roasted, in particular, the dark brown color was prominent.
[0117] 5. The seeds and other solids from the roasting step were ground using a grinder (e.g., a wet grinder, a crushing mill, a burr mill, an espresso grinder, a stone mill, or a jet mill) to a particle size of 350 μm or less (preferably 150 μm or less), and optionally sieved to remove unwanted material. For wet grinding, a fat or liquid oil (e.g., a vegetable fat such as cocoa butter or a cocoa butter equivalent) was added to the seeds before grinding, and then ground into a paste. A fat in an amount of 30 - 60% by weight was added to the roasted grape seeds and wet ground in the fat to produce a pasty wet-ground grape seed product. The wet grinding was carried out using a stone mill (e.g., a stone melanger), a colloid mill, a blade mill, or a corundum mill.
[0118] Example 6 - Processing of Seed Material (Roasting) The seed material was processed according to the following procedure.
[0119] 1. To remove husks, broken materials, and other products of agricultural origin (e.g., stones, skins, stems, and branches), the complete seeds were washed with machines such as destoners, scalping decks, suction channels, sizing decks, optical sorters, sieves, or combinations thereof. The target impurities at the end of the washing process were less than 0.5% w / w. To measure the impurities, a 1-kilogram sample of the washed complete seeds was visually inspected and hand-sorted to remove husks, broken materials, and other products that were not removed during the washing process. This yielded two samples that were hand-sorted and weighed. The impurities were reported as a percentage of the washed sample.
[0120] 2. After the washing step, the seeds were placed in a convection / conduction roaster to initiate the drying process.
[0121] 3. While stirring, the seeds were heated by convection and / or conduction to evaporate the water and dry the seeds. To facilitate this process, the temperature and air speed (if used) were increased.
[0122] 4. When the moisture content of the seeds reached less than 5% w / w, the roasting temperature was increased above 125°C (e.g., up to 200°C). The seeds were roasted using convection, conduction, or a combination of the two. For example, the dried seeds were roasted in a convection roaster at a temperature of 140°C to 200°C for 20 minutes to 2 hours to obtain roasted seeds. After roasting was complete, the seeds were observed to have turned dark brown and produced coffee-like sensory notes.
[0123] 5. Seeds and other solids from the roasting process were ground to a particle size of 350 μm or less (preferably 150 μm or less) using a grinder (e.g., wet grinder, crushing mill, bar mill, espresso grinder, stone mill, jet mill, etc.), and optionally sieved to remove unwanted materials. For wet grinding, a fat or liquid oil (e.g., a vegetable fat such as cocoa butter or a cocoa butter equivalent) was added to the seeds before grinding, and then ground into a paste. A fat in an amount of 30 - 60% by weight was added to the roasted grape seeds, and wet ground in the fat to produce a pasty wet ground grape seed product. The wet grinding was carried out using a stone mill (e.g., a stone melanger), a colloid mill, a blade mill, or a corundum mill.
[0124] Preparation of Example 7 - 60% Chocolate Product Chocolate was prepared using a standard method for most small bean - to - bar chocolates. Raw, screened (shell - removed) cocoa nibs from Peru were roasted in a 300°F high - convection oven at 100 g increments for 7 minutes. This formulation was based on 60.1% standard Barry Callebaut chocolate, which has high consumer acceptability and available compositional data. The recipe included the following. 22.7% by weight of non - fat cocoa solids 37.4% by weight of cocoa butter 39.9% by weight of sugar
[0125] Based on data showing the amount of fat in the cocoa nibs, this formulation was determined to have the following composition (by weight). 45.4% roasted nibs 14.7% additional cocoa butter (standard) 39.3% sugar (standard granulated sugar)
[0126] The complexes were mixed and milled for 16 hours using a stone mill (CocoaTown; Alpharetta, GA) with the pressure set to "high". The final particle size was 25 microns.
[0127] Based on the solids information, to mimic a pure chocolate formulation, a grape seed version of chocolate ("grape seed chocolate") was created with the following composition. 22.7 wt% grape seeds (dutched to pH 8.5 as a solution, dried, and roasted at 380°F for 30 minutes) 37.4 wt% cocoa butter 39.9 wt% sugar
[0128] The formulation was mixed and milled for 48 hours using a stone mill (Cocoatown) with the pressure set to "high". Since the seed material was harder, the grape seed chocolate required more milling to achieve a similar particle size. The final particle size ranged from 25 - 35 microns. For both the control chocolate and the grape seed chocolate, the particle size was measured multiple times during the milling process using a micrometer screw and a Hegman gauge, and by reading, an average particle size of approximately 25 microns was confirmed for both the control chocolate and the grape seed chocolate.
[0129] Since the chocolates were made to be compositionally identical, the grape seed chocolate was mixed with "real" chocolate in a 3:1 ratio to obtain a solids composition consisting of 75 wt% grape seeds and 25 wt% cocoa. Thus, 75% (by weight) of the cocoa solids were replaced with grape seeds.
[0130] The chocolate was tempered, hand - molded into bars, then fully cooled and removed from the mold. The chocolate bars were subjected to a sensory test at room temperature using the protocol described in Example 8.
[0131] Example 8 - Sensory Test For the sensory evaluation of chocolate containing grape seed extender compared to chocolate without grape seed extender, a panel of 5 trained descriptive panelists was used. The Flavor Profile Method (FPM; International Organization for Standardization (ISO) 6564; details can be found at https: / / www.iso.org / standard / 12966.html) was used to assess the intensity of chocolate aroma and flavor in a 60 (weight)% chocolate / grape seed product. Panel members individually evaluated the product and then had a group discussion to determine the consensus profile. It was not possible to refer to reference materials to help the group reach consensus if no consensus was obtained. For the conditions of the room where the test was conducted, refer to ISO 6658 (details can be found at https: / / www.iso.org / standard / 65519.html). The 7-point scale used included scores in the range of 0 - 3 as shown in Table 1 below.
[0132] (Table 1) Sensory Score Levels TIFF2025523059000002.tif46128
[0133] When the combined results were collected, these studies showed that 60 (weight)% chocolate and 75 (weight)% grape seed replacement products had the same sensory characteristics (Table 2).
[0134] (Table 2) Combined Sensory Scores TIFF2025523059000003.tif107149
[0135] Therefore, these data showed that replacing up to 75% of the cocoa solids with grape seed extender had favorable sensory results.
[0136] Example 9 - Viscosity Test (Productivity Enhancement) The above research showed that even when 75% of the cocoa solids (by weight) were replaced with grape seed extender, no flavor difference occurred. Further research showed that replacement of a smaller proportion of cocoa solids (2%) also imparted enhanced processability. Specifically, 2% of the solids in cocoa liquor (by weight) were replaced with grape seed liquor prepared with cocoa butter.
[0137] Except for using only fat and solids, the liquor was processed using a stone melanger as described above. For cocoa liquor, this meant that the processing mix was only nibs since solids and fat were already present. For grape seed liquor, grape seeds were mixed with cocoa butter at a solids ratio equal to that of cocoa nibs (47% solids, 53% fat). The liquor was given an equal particle size, 25 microns, as measured by a micrometer screw.
[0138] The viscosity of 100% cocoa nib liquor was measured, and the viscosity of 96% cocoa nib liquor with 4% grape seed liquor added to give a 2% cocoa solids replacement was also measured. For chocolate, when cocoa butter is present at a lower ratio (closer to that found in cocoa nibs), strong flow resistance can exist. However, since cocoa butter is costly, increasing the amount of cocoa butter to improve processability may not be ideal. Other additives (e.g., PGPR) can be used to enhance flow characteristics, but chocolate containing such additives may not be desirable to consumers.
[0139] The measurements were carried out using a Bostwick Consistometer and a Zahn Cup (ASTM D4212). The Bostwick Consistometer is an industry standard for measuring fluidity and consistency. The faster the product flows down the gradient of the consistometer, the lower the flow resistance. The product was measured at 140°F and the room was at 71.5°F. Thirteen marks on the Bostwick Consistometer were used as measurement points. The time for pure cocoa nib liquor to flow down the gradient was 1:04:06 (mm:ss:ms), while the time for the liquor containing 2% (by weight) grape seed solids was 00:13:55.
[0140] The Zahn Cup (ASTM D4212) is a measure often used in the dairy industry to measure the viscosity of materials. This device is used to measure the time it takes for the material to flow through a standardized hole in a cup. The Zahn Cup is similar to the Bostwick test in terms of information, but for applications where the chocolate needs to be made thinner to create a thin and uniform shell in a mold (e.g., shell mold forming), it provides additional information about the fluidity of the material. Here too, cocoa butter can be increased to ease these viscosity differences, but these studies have shown that the viscosity decreases significantly by including grape seed liquor to replace 2% (by weight) of the cocoa solids. Specifically, at 140°F for the product measured in a 71.5°F room, the time for pure cocoa nib liquor to pass through the Zahn Cup was 01:34 (mm:ss), while the time for the liquor containing 2% grape seed solids was 01:17. Therefore, grape seed liquor was successfully used as a processing aid to improve the fluidity of chocolate.
[0141] Collectively, the foregoing studies have shown that the use of the grape seed extender provided herein results in a chocolate product having the characteristics of traditional chocolate (e.g., taste, aroma, and viscosity) without increasing the cost of production. These results indicate that grape seeds can be used to replace cocoa solids, which provides cost reduction, supply chain stabilization, and enhanced processability.
[0142] Example 10 - Volatile Organic Compounds (VOCs) in Chardonnay Grape Seeds LC-MS was used to measure the levels of various compounds in Chardonnay grape seeds and reference chocolate according to the following method.
[0143] All analyses were performed on a Thermo Ultimate 3000 Ultra-Performance Liquid Chromatograph (UPLC) connected to a Thermo Scientific Q-Exactive high-resolution mass spectrometer (MS). XCalibur software was used for data acquisition, and the mass spectrometer parameters were as follows for all methods: Polarity: Positive mode or negative mode indicated for each method Resolution: 70,000 Scan range: 60 - 900 m / z for all methods except the lipid method, which was 134 - 2000 m / z Isolation window: 1.5 m / z MS / MS collision energy: 30
[0144] Preparation of Analytical Standards: Stock solutions for each compound were prepared in 50% methanol at a concentration of 1 mg / mL. Subsequently, each compound was serially diluted to create a 15-point standard curve in the range of 10 ng / mL to 20 μg / mL. Standard curves were run with combinations of 7 - 12 compounds from each category for each set, as long as there was no retention time overlap that would interfere with quantification. The retention time for each compound was pre-determined by running the analytical standard at 20 μg / mL dilution and identifying the compound based on the exact mass. In all cases, 5 μL of each standard mixture was injected into the MS through an autosampler and LC. Separation was performed on chromatographic columns specific to each compound class. Conditions for each chromatographic method, including the column, mobile phase, and gradient used for each method, are described below.
[0145] As shown in Tables 3A - D, several types of columns and different limits of detection (LOD) were used for different compounds.
[0146] (Table 3A) List of compounds quantified by each method in the Round 1 assay TIFF2025523059000004.tif145153
[0147] (Table 3B) LOD (pg / mL, ng / mL, or μg / mL) for standards quantified in the Round 1 assay TIFF2025523059000005.tif145149
[0148] (Table 3C) Additional LOD for quantified standards TIFF2025523059000006.tif63128
[0149] (Table 3D) Methods and LOD for detected compounds TIFF2025523059000007.tif129128TIFF2025523059000008.tif215124TIFF2025523059000009.tif252124
[0150] Quantification of amino acids and similar polar compounds: To assay polar compounds that can retain a positive charge, a HILIC (hydrophilic interaction liquid chromatography) column was used (Table 4). The mobile phase used with this column contained A: H2O + 5 mM ammonium acetate + 0.1% TFA (trifluoroacetic acid), and B: 90 / 10 ACN (acetonitrile) / H2O + 5 mM ammonium acetate + 0.1% TFA. The time for each chromatographic run was 27.5 minutes, and the column temperature was maintained at 40 °C. The column used was a Phenomenex Luna, 3 μm NH2, 100 Å, 150 × 2 mm (product #00F-4377-B0), and the guard column was a Phenomenex Security Guard Cartridge, NH2, 4 × 2 mm (#PRD-196870).
[0151] (Table 4) HILIC positive mode gradient conditions TIFF2025523059000010.tif40128
[0152] Quantification of sugars and sugar alcohols: The same HILIC column used for the quantification of amino acids was used for the quantification of sugars, but the MS polarity was run in negative mode (Table 5). The same mobile phase was used, but the gradient was slightly modified to aid retention. The column temperature was also kept at 50 °C for better peak shape and isobaric separation of sugars.
[0153] (Table 5) HILIC negative mode gradient conditions TIFF2025523059000011.tif51128
[0154] Quantification of Nonpolar Compounds: Since nonpolar compounds are retained on a long carbon chain under polar conditions, a C18 column was used to assay nonpolar compounds. This method was performed in both positive and negative modes depending on each compound's better ionization with either a positive or negative charge respectively. The mobile phase used for this method was A: H2O + 0.1% FA, and B: methanol, and the column temperature was maintained at 50 °C. The column used was Agilent Poroshell 120, EC-C18 2.7 μm, 3.0 × 100 mm (product #695975-302).
[0155] (Table 6) C18 Positive / Negative Mode Gradient Conditions TIFF2025523059000012.tif40128
[0156] Quantification of Organic Acids and Polar Compounds with Similar Charges: To examine organic acids, a charged C18 column was used. The gradient used for the organic method was the same as the C18 nonpolar method shown in Table 6. For this method, mobile phase B was modified to B: ACN + 0.1% FA. The column used was Phenomenex Luna Omega, 1.6 μm, PS C18 100 Å, 100 × 2.1 mm (product #00D-4752-AN).
[0157] Data Analysis: The data analysis method was developed by the XCalibur Processing Setup program, and the method was created for each LC method and for each standard cassette. For each standard, the mass and retention time of the compound were added, and a calibration level was applied for each standard. To calculate the concentration in the sample, the sample and standard for each run were processed together using XCalibur Quan software, and the concentration was calculated based on the calibration curve of each compound. The detection limit for each standard was determined by running each standard curve at a low level until it was no longer detected at all.
[0158] Quantification of organic acids: Since organic acids are retained on a charged stationary phase under polar conditions, a Synergi Hydro reversed-phase column was used to assay organic acids (Table 7). This method was carried out in negative ionization mode. The mobile phases used for this method were A: H2O + 0.1% FA, and B: acetonitrile + 0.1% FA, and the column temperature was maintained at 50 °C. The column used was a Phenomenex Synergi 2.5 μm Hydro RP, 100 Å, 100×2 mm (Product #00D - 4387 - B0).
[0159] (Table 7) Synergi Hydro negative mode gradient conditions TIFF2025523059000013.tif40128
[0160] A list of the compounds detected in Chardonnay grape seeds is shown in Table 8. Table 9 contains a list of the compounds detected in both grape seeds and reference chocolate.
[0161] (Table 8) Compounds detected in grape seeds TIFF2025523059000014.tif246160TIFF2025523059000015.tif211160TIFF2025523059000016.tif214160TIFF2025523059000017.tif195160
[0162] (Table 9) Compounds detected in grape seeds and reference chocolate TIFF2025523059000018.tif207143TIFF2025523059000019.tif150143
[0163] Example 11 - Comparison of the fiber and protein contents between grape seeds and cacao beans Complete grape seeds and cocoa beans were evaluated to determine the content of carbohydrates, fiber, protein, fat, moisture, and ash using the methods of the Association of Official Agricultural Chemists (AOAC). As shown in Table 10, these studies revealed that grape seeds and cocoa beans are similar in their content. Furthermore, both cocoa beans and grape seeds were found to have extremely high tannin content and also high flavonoid content.
[0164] (Table 10) TIFF2025523059000020.tif40149
[0165] Example 12 - Extender Produced from Non-Grape Seeds Experimental tests were conducted on other (non-grape) fruit seeds processed as described in Example 7 above. Specifically, a hedonic sensory test was then carried out using a blinded focus group (Table 11). These studies indicated that extenders derived from non-grape seeds are suitable for inclusion in chocolate products.
[0166] (Table 11) TIFF2025523059000021.tif101149
[0167] Example 13 - Method for Measuring Particle Size To measure the average particle size of the wet materials, a micrometer screw gauge was used, which included roasted and ground wet seeds, with added fat or liquid, and then wet ground into a paste, grape seed liqueur (wet ground grape seeds), control chocolate products such as 60.1% of the standard Barry Callebaut recipe chocolate of Example 7, and chocolate containing the extender of Example 7 (chocolate manufactured with grape seed extender or other seed extenders). To prepare the samples, aliquots were diluted 1:1 with neutral oil to break up the aggregates. The micrometer screw method utilizes a measuring stage with a dial gauge. The dial of the dial gauge was turned until the measuring stage was pressed against the opposite side of the gauge. The distance between the two surfaces, indicating the size of the largest particle on the stage, was accurately measured with the apparatus and reported in micrometers. The measurements were repeated and averaged to obtain the average particle size value.
[0168] For measuring the average particle size of wet materials, including roasted and ground wet seeds, grape seed liquor, with fat or liquid added, then wet ground seeds into paste, seeds with fat or liquid added after dry grinding, grape seed extender, berry seed extender, control chocolate product, chocolate containing extender, and other chocolate products, a Hegman gauge (grind meter) was used. To prepare the sample, an aliquot was diluted 1:1 with neutral oil to break up the aggregates. The grind meter has a base with calibrated grooves that can be made equal to the diameter of the particles. An aliquot of the diluted material was poured into the grooves. While moving from the larger end to the smaller end (i.e., from the deeper groove to the shallower groove) at a slight angle, a flat steel edge (scraper) was pressed against the grind meter. When the end of the gauge was reached, a pattern was observed in the grooves. Specifically, streaks indicated that the particle size was larger than the depth of the groove at that point. The position of the groove where the streaks were first formed indicated the upper limit of the distribution, and the position where 50 - 75% of the surface streaks were observed indicated the average particle size. The grind meter provided an indication of the particle size distribution in addition to the average particle size. The measurements were repeated to provide an average value of the particle size.
[0169] For particle size analysis of dry materials or dry solids-containing materials, including dry ground grape seeds, cranberry seeds, raspberry seeds, blueberry seeds, blackberry seeds, pomegranate seeds, and strawberry seeds, a RoTap was used. The RoTap uses a uniform rotational motion and tapping at the top of the sieve stack to determine the percentage of dry powder that falls within a specific mesh / micron size range and calculates the amount of material retained on each test sieve after operation of the RoTap machine. 300 - 1000 grams of dry material was placed on the top screen and the stack was closed. Then the machine was set to rotate for a certain time and the screen stack was tapped. At the end of the cycle, the distribution of the material between each screen was measured. Care was taken to avoid excessive oil in the material, which could cause clogging of the screens at finer mesh sizes. This process was repeated to obtain an average value of the particle size.
[0170] In some samples, laser diffraction and dynamic light scattering / laser diffraction were used to measure the particle size. The laser diffraction particle size analyzer is suitable for detailed analysis of a small amount (about 0.25 g). To measure the particle size of some samples of the material of the present invention, a Malvern® particle size analyzer (PSA) was used. In the PSA, a laser beam is passed through the dispersed sample, and the variation in the angular scattered light intensity is measured. Small particles have small scattering angles, and large particles have large scattering angles. Then, the Mie theory of light scattering is used to analyze the angular scattered intensity data in order to calculate the size of the particles that created the scattering pattern. The particle size is reported as the equivalent volume sphere diameter.
[0171] Figure 1 shows the particle size distributions of grape seed liquor, i.e., wet-milled grape seeds ground into a paste, and the cocoa-free dark chocolate product of the present invention, measured with a Malvern® laser diffraction PSA.
[0172] (Table 12) Particle sizes measured for wet-milled grape seeds and cocoa-free chocolate TIFF2025523059000022.tif39149
[0173] Table 12 shows the particle size measurements from Malvern (registered trademark) PSA. The wet milled grape seed sample is a sample of processed grape seeds wet milled to a desired final particle size. The wet milled grape seed sample was prepared from the seed material processed according to the procedure of Example 1. The cocoa-free dark chocolate samples (Cocoa-free dark chocolate 1 and Cocoa-free dark chocolate 2) are fully prepared and finished chocolates using the ground grape seeds prepared according to the procedure of Example 1 and also contain the standard chocolate ingredients of sugar and fat. The chocolate samples were prepared with a cocoa-free formulation, i.e., the cocoa butter and cocoa solids were completely replaced with non-cocoa ingredients. Compositionally, the chocolate samples contained (based on solids information) 10 - 20 wt% grape seeds, 30 - 55 wt% sugar, and 25 - 45 wt% cocoa butter substitute, 7 - 20 wt% oilseed meal, 0.25 - 0.75 wt% lecithin, and 0 wt% cocoa solids. The formulation was blended and milled for 48 hours using a stone melanger (CocoaTown (registered trademark)) with the pressure set at "high". During the milling process, the particle size was measured using a micrometer screw and a Hegman gauge, and the finished cocoa-free chocolate samples were analyzed by laser diffraction.
[0174] Referring to Table 12, the upper Dx values indicate the particle size measurements of the particles at the percentage indicated in parentheses. For example, Dx(90) indicates the particle size of 90% of the particles such that 90% are below the stated particle size.
[0175] Dynamic light scattering / laser diffraction is an alternative analytical method for measuring particle size. In this method, two complementary devices (dynamic light scattering; laser diffraction) provide highly accurate readings. This method uses a very small amount of sample that is accurately diluted via an automated device. Once the dilution is complete, a laser passes through the sample. Based on the diffraction pattern from the diluted material, the machine provides an accurate measurement of the particle size distribution. This method can be used for chocolate mass as well as dry materials due to the flexibility of the equipment.
[0176] Dynamic light scattering / laser diffraction (DLS / LD) analysis was obtained for three finished chocolates that did not use cocoa solids, namely cocoa-free chocolate in which cocoa solids and cocoa butter were completely replaced by non-cocoa ingredients. The cocoa-free dark chocolate sample was a fully prepared and finished chocolate using ground grape seeds prepared according to the procedure of Example 1 and also contained standard chocolate ingredients such as sugar and fat. The chocolate sample was prepared with a cocoa-free formulation that did not contain cocoa-derived ingredients, i.e., cocoa butter and cocoa solids were completely replaced by non-cocoa ingredients. Compositionally, the chocolate sample contained (based on solids information) 10 - 20 wt% grape seeds, 30 - 55 wt% sugar, 25 - 45 wt% cocoa butter substitute, 7 - 20 wt% oilseed meal, 0.25 - 0.75 wt% lecithin, and 0 wt% cocoa solids. The formulation was mixed and blended for 30 minutes at 35°C and milled for 48 hours using a stone melanger (CocoaTown®) with the pressure set to "high".
[0177] (Table 13) Particle size of cocoa-free dark chocolate using DLS / LD TIFF2025523059000023.tif39149
[0178] Table 13 shows the measured particle sizes for three finished dark chocolate samples manufactured from the components of crushed grape seeds, sugar, and fat. Similar to the table showing the laser diffraction data obtained using Malvern® technology, the upper Dx values indicate the particle size measurements of the percentage of particles noted within parentheses. The average value of the particle sizes on the right side of the table is the mean of the distribution and is very similar to the micrometer readings of the samples.
[0179] Figure 2 also shows further statistical analysis of the samples, including the standard deviation and total span that indicate the extent of the width of the distribution in the samples. Specifically, the samples were dispersed in water and vortexed for 30 seconds prior to measurement to obtain an obscuration of 12 - 13%. The samples were then sonicated for 30 minutes (at 50w) before and during measurement. Tight particle sizes are preferred for chocolate and result in a smoother mouthfeel. This particular sample preparation utilizes sonication to prevent the formation of sample aggregates during measurement. Such aggregates can cause misrepresentation of larger particle sizes.
[0180] Other aspects The invention has been described with its detailed description, but it should be understood that the above description is for illustrative purposes of the invention and not for limiting the scope of the invention defined by the scope of the appended claims. Other aspects, advantages, and modifications are also included within the scope of the following claims.
Claims
1. A composition consisting essentially of roasted and ground fruit seeds.
2. The composition according to claim 1, wherein the ground fruit seeds have a particle size of less than 350 microns.
3. The composition according to claim 1 or claim 2, wherein the fruit seeds are grape seeds.
4. The composition according to claim 3, wherein the grape seeds are selected from table grapes, Concord, Niagara, Chardonnay, Sauvignon Blanc, Muscat, Sultana, Riesling, Pinot Gris, Pinot Grigio, Cabernet Sauvignon, Merlot, Pinot Noir, Shiraz, Albariño, Malbec, Grüner Veltliner, Solaris, Zinfandel, Cabernet Franc, Tempranillo, Carmenère, Mataro, Sangiovese, Regent, Black Muscat, Chasselas, Wild Grape, Nebbiolo, Montepulciano, Gewürztraminer, Barbera, Schönburger, Carignan, Semillon, Gamay, Petit Verdot, Trebbiano, Sancerre, and any combination thereof.
5. The composition according to claim 1 or claim 2, wherein the fruit seeds are selected from cranberries, raspberries, blueberries, strawberries, blackberries, pomegranates, kiwis, watermelons, honeydews, cantaloupes, papayas, passion fruits, star fruits, tomatoes, tomatillos, dragon fruits, guavas, loquats, calamansi, pumpkins, squashes, okras, cucumbers, bell peppers, eggplants, pears, apples, cherimoyas, pineapples, quince, loquats, dates, fenugreek, and any combination thereof.
6. The composition according to any one of claims 1 to 5, wherein the ground fruit seeds have a particle size of less than 250 microns.
7. The composition according to any one of claims 1 to 5, wherein the ground fruit seeds have a particle size of less than 150 microns.
8. An ingestible product comprising a bulking agent consisting essentially of roasted and ground fruit seeds.
9. The ingestible product according to claim 8, wherein the ground fruit seeds have a particle size of less than 350 microns.
10. The ingestible product according to claim 8 or claim 9, which is chocolate.
11. wherein the chocolate comprises from about 0.01 to about 35% by weight of said bulking agent; from about 20 to about 55% by weight of cocoa butter; from about 20 to about 60% by weight of sugar; and optionally from about 0.5 to about 25% by weight of cocoa solids and is an ingestible product according to claim 10.
12. wherein the chocolate comprises about 17.5% by weight of said bulking agent; about 37.5% by weight of cocoa butter; about 40% by weight of sugar; and optionally about 5% by weight of cocoa solids and is an ingestible product according to claim 10.
13. An ingestible product according to any one of claims 8 to 12, wherein the fruit seed is a grape seed.
14. An ingestible product according to claim 13, wherein the grape seed is selected from table grapes, Concord, Niagara, Chardonnay, Sauvignon Blanc, Muscat, Sultana, Riesling, Pinot Grigio, Pinot Gris, Cabernet Sauvignon, Merlot, Pinot Noir, Shiraz, Albariño, Malbec, Grenache, Solaris, Zinfandel, Cabernet Franc, Tempranillo, Carmenère, Mataro, Sangiovese, Regent, Black Muscat, Chasselas, Wild Grape, Nebbiolo, Montepulciano, Gewürztraminer, Barbera, Schönburger, Carignan, Semillon, Gamay, Petit Verdot, Trebbiano, Sancerre, Grüner Veltliner, Silvaner, Petit Syrah, Grenache Blanc and combinations thereof.
15. An ingestible product according to any one of claims 8 to 12, wherein the fruit seed is selected from cranberries, raspberries, blueberries, strawberries, blackberries, pomegranates, kiwis, watermelons, honeydews, cantaloupes, papayas, passion fruits, star fruits, tomatoes, tomatillos, dragon fruits, guavas, prickly pears, calamansi, pumpkins, squashes, okras, cucumbers, bell peppers, eggplants, persimmons, apples, cherimoyas, pineapples, quince, loquats, dates, or fenugreek and combinations thereof.
16. An ingestible product according to any one of claims 8 to 15, wherein the ground fruit seed has a particle size of less than 250 microns.
17. An ingestible product according to any one of claims 8 to 15, wherein the ground fruit seeds have a particle size of less than 150 microns.
18. A method for producing a substitute for dry cocoa solids from non-cocoa seeds, comprising: (a) treating a plurality of non-cocoa fruit seeds with a chemical solution and / or an enzyme solution, thereby producing treated seeds; (b) reducing the water content of the treated seeds to 25% w / w or less of the treated seeds, thereby producing dried seeds; (c) roasting the dried seeds, thereby producing roasted seeds; and (d) grinding the roasted seeds, thereby producing a ground seed composition effective as a substitute for dry cocoa solids.
19. A method for producing a chocolate product containing a bulking agent prepared from non-cocoa seeds, comprising: (a) treating a plurality of non-cocoa fruit seeds with a chemical solution and / or an enzyme solution, thereby producing treated seeds; (b) reducing the water content of the treated seeds to 25% w / w or less of the treated seeds, thereby producing dried seeds; (c) roasting the dried seeds, thereby producing roasted seeds; and (d) grinding the roasted seeds, thereby producing a ground seed composition used as all or part of the bulking agent.
20. The method according to claim 18 or claim 19, wherein the plurality of non-cocoa fruit seeds are washed before step (a) to remove impurities such as husks, broken materials, stones, skins, stems, and / or branches.
21. The method according to claim 20, wherein the plurality of non-cocoa fruit seeds are washed using a destoner, a scalping deck, a suction channel, a sizing deck, an optical sorter, a sieve, or a combination thereof such that the impurities are less than 0.5% w / w of the seeds.
22. The method according to any one of claims 18 to 21, wherein step (a) comprises using a chemical solution comprising a caustic agent (e.g., sodium hydroxide, potassium hydroxide, sodium carbonate, calcium carbonate, calcium hydroxide, potassium hydrogen carbonate, iodine, or a combination thereof), an acidulant (e.g., acetic acid, adipic acid, citric acid, fumaric acid, lactic acid, malic acid, phosphoric acid, and tartaric acid, glucono delta lactone, or a combination thereof), and / or an oxidizing agent (e.g., hydrogen peroxide).
23. The method according to claim 22, wherein the treated seeds are treated with the chemical solution for 30 minutes to 2 hours while being stirred at 60°C to 150°C (e.g., 75°C to 100°C) so that the treated seeds have a pH of 5.5 to 10.5 (e.g., 8 to 10).
24. The method according to any one of claims 18 to 23, wherein step (a) comprises using an enzyme solution comprising one or more enzymes including cellulase, tannase, pectinase, xylanase, and / or hemicellulase, preferably cellulase and / or hemicellulose, in an aqueous solution.
25. The method according to claim 24, wherein the seeds are treated with the enzyme solution for 30 minutes to 2 hours while being stirred.
26. The method according to any one of claims 18 to 25, wherein step (a) comprises treating the seeds with the chemical solution and / or the enzyme solution by immersion, spraying, boiling, stirring, coating, or a combination thereof.
27. The method according to any one of claims 18 to 26, wherein step (a) comprises treating the seeds with both the chemical solution and the enzyme solution simultaneously or sequentially.
28. The method according to any one of claims 18 to 27, wherein step (b) comprises reducing the water content of the treated seeds to 20% w / w, 15% w / w, 10% w / w, 6% w / w, or less of the treated seeds.
29. The method according to any one of claims 18 to 28, wherein step (c) comprises roasting the dried seeds at 125°C to 200°C, preferably 140°C to 200°C or 150°C to 175°C, for 20 minutes to 2 hours.
30. The method according to any one of claims 18 to 29, wherein the water content of the roasted seeds is less than 2% w / w of the roasted seeds.
31. The method according to any one of claims 18 to 30, wherein step (d) comprises using one or more dry grinding techniques and / or one or more wet grinding techniques to produce a ground seed composition.
32. The method according to any one of claims 18 to 31, wherein step (d) comprises using a wet grinder (e.g., a stone mill, a colloid mill, a blade mill, or a corundum mill) to grind the roasted seeds together with a fat or a liquid oil.
33. The method according to claim 32, wherein the fat or liquid oil is in an amount of 30 to 60% by weight of the roasted seeds.
34. The method according to any one of claims 18 to 33, wherein step (d) comprises grinding the roasted seeds to a particle size of less than about 350 μm.
35. The method according to any one of claims 18 to 33, wherein step (d) comprises grinding the roasted seeds to a particle size of less than about 250 μm or less than about 150 μm.
36. A method for producing a substitute for dry cocoa solids from non-cocoa seeds, comprising: (a) a step of washing a plurality of non-cocoa fruit seeds to remove impurities, thereby producing washed seeds; (b) a step of roasting the washed seeds at 125°C to 200°C, preferably 140°C to 200°C, for 20 minutes to 2 hours, thereby producing roasted seeds; and (c) a step of grinding the roasted seeds, thereby producing a ground seed composition that is effective as a substitute for dry cocoa solids.
37. A method for producing a chocolate product containing a bulking agent prepared from non-cocoa seeds, comprising: (a) a step of washing a plurality of non-cocoa fruit seeds to remove impurities, thereby producing washed seeds; (b) a step of roasting the washed seeds at 125°C to 200°C, preferably 140°C to 200°C, for 20 minutes to 2 hours, thereby producing roasted seeds; and (c) a step of grinding the roasted seeds, thereby producing a ground seed composition that is used as all or part of the bulking agent.
38. The method according to claim 36 or claim 37, further comprising reducing the water content of the washed seeds before step (b).
39. The method according to any one of claims 36 to 38, wherein step (c) comprises using a wet grinder (for example, a stone mill, a colloid mill, a blade mill, or a corundum mill) to grind the roasted seeds together with a fat or a liquid oil, and the fat or the liquid oil is in an amount of 30 to 60% by weight of the roasted seeds.
40. The method according to any one of claims 36 to 39, wherein step (d) comprises grinding the roasted seeds to a particle size of less than about 350 μm, less than about 250 μm, or less than about 150 μm.
41. The method according to any one of claims 19 to 35 and claims 37 to 40, wherein the chocolate product further comprises cocoa butter, sugar, and optionally cocoa solids.
42. The method according to any one of claims 19 to 35 and claims 37 to 40, wherein the chocolate product further comprises a substitute, replacement, or equivalent (CBE) of cocoa butter, sugar, and optionally cocoa solids, seed meal, and / or lecithin.