US20050214425A1 - Sugar substitute prepared with nutritive and high-intensity sweeteners - Google Patents

Sugar substitute prepared with nutritive and high-intensity sweeteners Download PDF

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Publication number
US20050214425A1
US20050214425A1 US10/807,067 US80706704A US2005214425A1 US 20050214425 A1 US20050214425 A1 US 20050214425A1 US 80706704 A US80706704 A US 80706704A US 2005214425 A1 US2005214425 A1 US 2005214425A1
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US
United States
Prior art keywords
composition
sucralose
sucrose
layer
binder
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Abandoned
Application number
US10/807,067
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English (en)
Inventor
Roma Vazirani
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Johnson and Johnson Consumer Inc
Original Assignee
McNeil PPC Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by McNeil PPC Inc filed Critical McNeil PPC Inc
Priority to US10/807,067 priority Critical patent/US20050214425A1/en
Assigned to MCNEIL-PPC, INC. reassignment MCNEIL-PPC, INC. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: VAZIRANI, ROMA
Priority to CNA2005800093950A priority patent/CN1934277A/zh
Priority to MXPA06010990A priority patent/MXPA06010990A/es
Priority to AU2005235983A priority patent/AU2005235983A1/en
Priority to EP05724906A priority patent/EP1730316A1/fr
Priority to CA002560757A priority patent/CA2560757A1/fr
Priority to BRPI0509097-0A priority patent/BRPI0509097A/pt
Priority to RU2006137296/13A priority patent/RU2006137296A/ru
Priority to JP2007504984A priority patent/JP2007530038A/ja
Priority to PCT/US2005/007467 priority patent/WO2005103304A1/fr
Priority to ARP050101119A priority patent/AR048438A1/es
Publication of US20050214425A1 publication Critical patent/US20050214425A1/en
Priority to IL178245A priority patent/IL178245A0/en
Abandoned legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C13SUGAR INDUSTRY
    • C13BPRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
    • C13B50/00Sugar products, e.g. powdered, lump or liquid sugar; Working-up of sugar
    • C13B50/002Addition of chemicals or other foodstuffs
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L27/00Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
    • A23L27/30Artificial sweetening agents
    • A23L27/33Artificial sweetening agents containing sugars or derivatives
    • A23L27/37Halogenated sugars
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23PSHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
    • A23P10/00Shaping or working of foodstuffs characterised by the products
    • A23P10/30Encapsulation of particles, e.g. foodstuff additives
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00Food compositions, function of food ingredients or processes for food or foodstuffs

Definitions

  • the present invention relates generally to high-intensity sweeteners. More particularly, the invention relates to granular sweetener compositions including a mixture of a nutritive sweeter and a high-intensity sweetener, in a form that minimizes separation of these components during shipping and handling.
  • Synthesis of sucralose is technically challenging because of the need to selectively replace specific hydroxyl groups with chlorine atoms, while preserving other hydroxyl groups including a highly reactive primary hydroxyl group. Numerous approaches to this synthesis have been developed. See, for example, U.S. Pat. No. 4,362,869; U.S. Pat. No. 4,826,962; U.S. Pat. No. 4,980,463; and U.S. Pat. No. 5,141,860, which are expressly incorporated in this document by reference.
  • Sucralose may be purified by crystallizing from water to form needle-shaped crystals, as described for example in U.S. Pat. No. 4,343,934; U.S. Pat. No. 4,950,746, U.S. Pat. No. 4,977,254; U.S. Pat. No. 4,980,463; U.S. Pat. No. 5,136,031; U.S. Pat. No. 5,498,709; and U.S. Pat. No. 5,530,106. Many of these crystals typically have a length-to-diameter (“L/D”) ratio ranging from about 4:1 to about 10:1, and in some cases even higher. Typically, many such needles are broken, which produces undesirable dust.
  • L/D length-to-diameter
  • the sweetener it is desirable for the sweetener to contain some amount of a sugar (typically sucrose, commonly referred to as table sugar) and some amount of a high-intensity sweetener.
  • a sugar typically sucrose, commonly referred to as table sugar
  • sucralose typically has a needle form, as noted above.
  • mixtures of these two components may separate to some degree during shipping and handling, resulting in unpredictable levels of sweetening when the consumer dispenses the product.
  • This result may be of particular importance in formulating certain popular products in which one half teaspoon of a sweetener is made mostly of sucrose with a small amount of a non-nutritive sweetener (such as sucralose), and has the same sweetening power as a full teaspoon of pure sucrose.
  • a non-nutritive sweetener such as sucralose
  • the present invention provides a sweetener composition, the composition comprising granules comprising, consisting of, or consisting essentially of (a) a core including a nutritive sweetener, and (b) on the core, a layer including sucralose.
  • the invention provides a method of making a sweetener composition.
  • the method includes the steps of (a) providing a plurality of granular cores each comprising, consisting of, or consisting essentially of sucrose; and (b) forming on the granular cores a layer comprising, consisting of, or consisting essentially of sucralose.
  • the invention provides a sweetener composition made by the method set forth in the preceding paragraph. It is to be understood that both the foregoing general description and the following detailed description are exemplary, but are not restrictive, of the invention.
  • high intensity sweetener and “non-nutritive sweetener” are used interchangeably and have the same meaning as those skilled in the art ascribe to such terms, presently or in the future.
  • the sweetener compositions of the invention include granules, which in turn have a core and a layer deposited on such core.
  • the core includes at least one nutritive sweetener, and the layer deposited on the core includes sucralose.
  • the nutritive sweetener(s) in the cores of the compositions of this invention may include, as non-limiting examples, sucrose, fructose, invert sugar, dextrose, maltodextrin, sugar alcohols, and combinations of any of these.
  • sucrose alone is used, and thus the core consists essentially of sucrose.
  • consists essentially of it is meant that no other ingredients are purposefully added to the core that change the sweetness profile of the core.
  • Sources of sucrose suitable for use according to the present invention include any commonly available source, such as, for example, beet sugar and cane sugar. They may include white sugar or brown sugar.
  • cores of a relatively uniform size in order to provide a more even distribution of sucralose on the cores.
  • a uniform size may be beneficial because the use of cores having a wide distribution of sizes may result in the smaller particles including a higher percentage by weight of sucralose, and thus any settling and separation of small from large particles may result in uneven sweetness within a sample.
  • Commercially available granules from any of a wide variety of sources known in the art may be used, and are typically sieved before use in order to achieve a relatively uniform size distribution.
  • the cores are therefore essentially solid, and are typically of such a size and shape that they resemble common table sugar.
  • a typical (but non-limiting) size distribution for the cores is as follows: no more than 3% retained on a 20-mesh sieve, a minimum of 8% (cumulative) retained on a 40-mesh sieve, and no more than 10% passing through a 100-mesh sieve.
  • the layer deposited on the core may contain (other than materials of no essential significance) only sucralose, or it may include sucralose in combination with one or more binders and/or with other non-nutritive sweeteners.
  • suitable non-nutritive sweeteners include, but are not limited to, saccharin, acesulfame-K, cyclamate, stevia, neotame, alitame, aspartame, and combinations of such sweeteners.
  • Binders suitable for use according to the invention include, but are not limited to, nutritive sweeteners, such as those mentioned above, including mixtures of them.
  • Other suitable binders include, as non-limiting examples, maltose, glucose, polyols (e.g., sugar alcohols, such as erythritol and sorbitol), modified food starches, gum, inulin or hydrolyzed inulin, maltodextrin, and combinations of these examples.
  • the binder will include sucrose, and may contain (other than materials of no essential 15 significance) only sucrose.
  • sucralose constitutes between about 30 wt % and about 50 wt % of the layer, with one or more binders making up the balance.
  • sucralose is present in an amount of between about 0.1 wt % and about 50 wt % of the sweetener composition.
  • essentially all of the composition contains (other than materials in trace amounts) only granules having a core with a sucralose-containing layer deposited on the core, with the composition containing between about 0.1 wt % and about 0.50 wt % sucralose, the remainder containing (other than materials of no essential significance) only sucrose.
  • the resulting sweetener composition has a sweetness equivalence of one-half teaspoon equal to a full teaspoon of sucrose.
  • the sweetener composition may contain between about 1.0 wt % and about 50 wt % sucralose, with the rest containing (other than materials of no essential significance) only sucrose.
  • Such a material may be blended with sucrose (in a ratio depending on the content of sucralose in the material) to provide a product with between about 0.1 wt % and about 0.5 wt % of sucralose overall.
  • a blended product is another embodiment of the invention.
  • Other weight percent loadings of sucralose will be apparent to persons skilled in the art, and the invention is not restricted to any particular proportions of sucralose and sucrose on any given granule or fraction of granules.
  • the layer including sucralose may be composed of any of a number of formulations.
  • the layer may be provided, for example, by applying a dispersion (which may be a solution) including sucralose in an appropriate volatile carrier, such as water, to the granular cores and evaporating the volatile carrier. Methods of applying such coatings will be discussed below.
  • the dispersion that is applied to the cores contains only sucralose and the carrier, and the layer thus produced contains (other than materials of no essential significance) only sucralose.
  • a binder is included in the sucralose-containing dispersion.
  • the sucralose may be dispersed in that binder.
  • the layer may contain (other than materials of no essential significance) only a solid solution of sucralose and binder, by which it is meant that the sucralose is dissolved in the binder or a component of the binder (if the binder has more than one component), and/or the binder (or a component of the binder) is dissolved in the sucralose.
  • the layer may also, or instead, have particles containing (other than materials of no essential significance) only sucralose dispersed within it.
  • the layer may be essentially continuous, and it may cover essentially the entire surface of a given granule, or it may include isolated patches of layer composition, or there may be an at least partially interconnected network of regions of layer composition on the cores.
  • the material in the layer is essentially solid, meaning that there are few or no hollows or voids in the layer, with the obvious exception that the entire layer itself may be hollow in the sense that it may constitute a continuous shell around the core.
  • Sweetener compositions according to the invention typically have a bulk density approximately equal to that of common table sugar.
  • the bulk density may be in the range of about 0.7 to 0.9, typically between 0.8 and 0.86.
  • sweetener compositions according to the invention include granules with a core and a layer.
  • the composition may contain (other than materials of no essential significance) only such granules, or it may include the granules mixed with other materials.
  • Such other materials may include non-sweet diluents and/or nutritive sweeteners.
  • the granules are mixed with a nutritive sweetener including, or containing (other than materials of no essential significance) only sucrose.
  • the sweetener composition includes about 10 wt % of a granular material including a core and a layer on the core, with the rest of the composition containing (other than materials of no essential significance) only granules of uncoated sucrose.
  • the sucralose in the granules having a core and a layer constitutes between about 1 wt % and 5 wt % of those granules.
  • the layer contains sucralose and sucrose, which acts as a binder, and the core is sucrose as well.
  • a composition may have storage stability, as measured by a 14-day accelerated aging test, greater than that of compositions in which the sucralose is not provided in a layer on a sucrose core.
  • 14-day accelerated aging test as used for the purposes of this invention, is described in detail in the Examples section, and measures the color of the material according to the Hunter Lab® method, which is well known in the art.
  • Sweetener compositions according to the invention have good stability as indicated by this test, and may for example have a Hunter “a” value no greater than 0.2 units, more typically no greater than 0.1 units, higher than the Hunter “a” value of the composition before aging. They may have a Hunter “b” value that is no greater than 1.0 units higher than the “b” value of the composition prior to aging.
  • the enhanced color stability of sweetener compositions according to the invention may result from the dispersion of the sucralose into small domains in the layer residing on the cores.
  • These small domains may be small particles containing (other than materials of no essential significance) only sucralose, or the domains may be of a molecular size, in other words, a solid solution of sucralose in a binder component, or vice versa. It is believed that, for either or both of these reasons, dispersion or dilution of the sucralose results in increased stability of the sweetener composition.
  • the layer including sucralose and (optionally) a binder may be formed on the cores by any of a number of methods known in the art. Such methods include, as non-limiting examples, spray-drying and fluidized bed drying.
  • One particularly suitable method of forming the layer is by pan-coating, which may be used in either batch mode or continuous mode.
  • Equipment suitable for pan-coating of granules such as those of the present invention is well-known in the pharmaceutical compounding art, and is available from a variety of manufacturers.
  • a typical machine has a rotating pan in which the granular cores tumble.
  • a spray nozzle is typically placed through an opening in the drum, and a mixture of the sucralose-containing layer composition in a volatile carrier is sprayed onto the granular cores.
  • a wave is created as the pan turns, and the granules tumble in a wave form.
  • the coating material slowly builds up on the granules, which are dried to form the layer.
  • the coating operation may be performed in a single step, with drying being performed either concurrently or subsequently to the spraying on of the aqueous mixture. Typically, a series of coating/drying cycles is performed, until the desired layer weight is produced.
  • particles including sucralose may be introduced after spraying but before drying is complete, so that the particles adhere to the granules. This may reduce the time required to provide the desired amount of sucralose, by reducing the drying time per unit of sucralose added. Drying may be performed by any mechanism known in the art, including for example the application of a stream of air or other gas, such as nitrogen, and/or warming the contents of the rotating pan. For example, it has been found suitable to warm the contents of the rotating pan to between about 38° C. and 93° C., more typically between 52° C. and 66° C., because drying within this temperature range has been found to be helpful in providing a product with good accelerated aging stability.
  • the sucralose to be incorporated in the layer is added in the form of an aqueous mixture, optionally containing other volatile carriers.
  • suitable volatile materials such as methanol, ethanol, isopropyl alcohol, and ethyl acetate.
  • water is the only carrier and the aqueous mixture also contains sucrose as a binder.
  • the binder contains (other than materials of no essential significance) only sucrose.
  • substantially all of the sucralose to be used in forming the layer is dissolved in the aqueous mixture.
  • a mixture may for example include between 20 wt % and 60 wt % of water, between 15 wt % and 55 wt % of sucrose, and between 15 wt % and 35 wt % of sucralose.
  • the mixture includes between 35 wt % and 45 wt % of water, between 31 wt % and 41 wt % of sucrose, and between 18 wt % and 28 wt % of sucralose.
  • a sweetener composition according to the invention was prepared as follows. A mixture of 23.2 parts by weight of sucralose, 54.2 parts by weight of a 67.7 wt % aqueous sucrose solution, and 22.6 parts by weight of water was mixed at 70° C. until all components were dissolved. The resulting coating composition contained 23.2 wt % of sucralose, 36.8 wt % of sucrose, and 40.0 wt % of water.
  • Extra fine sugar (sucrose) was sieved through a 52T screen and charged to a 48-inch Stokes coating pan.
  • the contents of the coating pan were heated to approximately 54° C., and several applications of coating composition were applied by a sprayer operated at an average spray pressure of 84 psi, using a No. 30 spray tip equipped with an inline filter.
  • the product was heated until dry (which was indicated by an operator squeezing the product in a fist, to make sure it did not clump) before the next coating was applied.
  • a stainless steel hoop was used to agitate the bed of granular material.
  • the average bed temperature was approximately 57° C.
  • the resulting product was sieved through an 18T sieve and had a sucralose content of 2.2 wt %.
  • This concentrated product was dry-blended in a weight ratio of 1 part out of 10 with extra fine sugar (sieved as described above) using a rotary tote blender to provide a product having a sucralose content of 0.22 wt %.
  • This material had a composition such that one half teaspoon had the sweetness equivalence of a full teaspoon of sucrose.
  • a sweetener composition including a simple mechanical mixture of sucrose and sucralose was prepared as follows. A composition containing 0.22% micronized sucralose and 99.78% extra fine sugar was blended for 5 minutes using a TURBULA® Shaker-Mixer—Model T2F, available from Glen Mills Inc. of Clifton, N.J. Accelerated aging of the samples prepared in Examples 1 and 2 was performed as follows. The sweetener composition was maintained at 50° C. and sampled after a given number of days. The color of a dry sample of the composition was evaluated in a 10-mm cuvette by the Hunter Labs method.
  • samples having an “a” value greater than zero have a net red color component; those samples with a negative “a” value have a net green color component.
  • samples having a Hunter “b” value greater than zero have a net yellow color component; those with a negative “b” value have a net blue color component.
  • Samples having both “a” and “b” values equal to zero are colorless. Samples having high “L” values are brighter than those with low values.

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  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Proteomics, Peptides & Aminoacids (AREA)
  • Health & Medical Sciences (AREA)
  • Nutrition Science (AREA)
  • Biochemistry (AREA)
  • Organic Chemistry (AREA)
  • Seasonings (AREA)
  • Medicinal Preparation (AREA)
US10/807,067 2004-03-23 2004-03-23 Sugar substitute prepared with nutritive and high-intensity sweeteners Abandoned US20050214425A1 (en)

Priority Applications (12)

Application Number Priority Date Filing Date Title
US10/807,067 US20050214425A1 (en) 2004-03-23 2004-03-23 Sugar substitute prepared with nutritive and high-intensity sweeteners
PCT/US2005/007467 WO2005103304A1 (fr) 2004-03-23 2005-03-08 Substitut de sucre prepare avec des edulcorants nutritifs de forte intensite
BRPI0509097-0A BRPI0509097A (pt) 2004-03-23 2005-03-08 substituto de açúcar preparado com adoçantes nutritivos e de alta intensidade
MXPA06010990A MXPA06010990A (es) 2004-03-23 2005-03-08 Sustituto de azucar preparado con edulcorantes nutritivos y de alta intensidad.
AU2005235983A AU2005235983A1 (en) 2004-03-23 2005-03-08 Sugar substitute prepared with nutritive and high-intensity sweeteners
EP05724906A EP1730316A1 (fr) 2004-03-23 2005-03-08 Substitut de sucre prepare avec des edulcorants nutritifs de forte intensite
CA002560757A CA2560757A1 (fr) 2004-03-23 2005-03-08 Substitut de sucre prepare avec des edulcorants nutritifs de forte intensite
CNA2005800093950A CN1934277A (zh) 2004-03-23 2005-03-08 用营养性和高甜度的增甜剂制备的糖替代物
RU2006137296/13A RU2006137296A (ru) 2004-03-23 2005-03-08 Заменитель сахара, полученный с питательными и высокоинтенсивными подсластителями
JP2007504984A JP2007530038A (ja) 2004-03-23 2005-03-08 栄養甘味料と強力な甘味料とで調製された砂糖代用品
ARP050101119A AR048438A1 (es) 2004-03-23 2005-03-22 Sustituto del azucar preparado con edulcorantes nutritivos y de alta intensidad
IL178245A IL178245A0 (en) 2004-03-23 2006-09-21 Sugar substitute prepared with nutritive and high-intensity sweeteners

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US10/807,067 US20050214425A1 (en) 2004-03-23 2004-03-23 Sugar substitute prepared with nutritive and high-intensity sweeteners

Publications (1)

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US20050214425A1 true US20050214425A1 (en) 2005-09-29

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US10/807,067 Abandoned US20050214425A1 (en) 2004-03-23 2004-03-23 Sugar substitute prepared with nutritive and high-intensity sweeteners

Country Status (12)

Country Link
US (1) US20050214425A1 (fr)
EP (1) EP1730316A1 (fr)
JP (1) JP2007530038A (fr)
CN (1) CN1934277A (fr)
AR (1) AR048438A1 (fr)
AU (1) AU2005235983A1 (fr)
BR (1) BRPI0509097A (fr)
CA (1) CA2560757A1 (fr)
IL (1) IL178245A0 (fr)
MX (1) MXPA06010990A (fr)
RU (1) RU2006137296A (fr)
WO (1) WO2005103304A1 (fr)

Cited By (11)

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US20060210698A1 (en) * 2005-03-18 2006-09-21 Nehmer Warren L Granular sucralose
GB2436514A (en) * 2006-03-28 2007-10-03 Tate & Lyle Plc A granulated sugar product
US20070264403A1 (en) * 2006-05-11 2007-11-15 Nehmer Warren L Sparkling agglomerated sweetener, and method of making it
US20100055255A1 (en) * 2008-08-26 2010-03-04 John Doyle Sweetener Compositions and Methods for Their Manufacture
US20110059218A1 (en) * 2008-05-09 2011-03-10 Cargill Incorporated Sweetener, methods of preparing sweetener and applications thereof
US8017168B2 (en) 2006-11-02 2011-09-13 The Coca-Cola Company High-potency sweetener composition with rubisco protein, rubiscolin, rubiscolin derivatives, ace inhibitory peptides, and combinations thereof, and compositions sweetened therewith
US9101160B2 (en) 2005-11-23 2015-08-11 The Coca-Cola Company Condiments with high-potency sweetener
US20160295893A1 (en) * 2013-11-13 2016-10-13 Tate & Lyle Technology Limited High intensity sweetener composition
US9833015B2 (en) 2014-06-13 2017-12-05 NutraEx Food Inc. Sweetener with imbedded high potency ingredients and process and apparatus for making the sweetener
US20180116265A1 (en) * 2016-10-31 2018-05-03 Morris IP Holdings LLC Blended high-intensity sweetener composition
US12016357B2 (en) 2015-05-20 2024-06-25 Cargill, Incorporated Glycoside compositions

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US20060068058A1 (en) * 2004-09-30 2006-03-30 Cadbury Adams Usa Llc Thermally stable, high tensile strength encapsulation compositions for actives
EP2100519A1 (fr) * 2008-03-04 2009-09-16 Tiense Suikerraffinaderij N.V. Particule contenant un édulcorant à haute intensité, procédé de préparation et utilisation
WO2012007961A2 (fr) * 2010-07-11 2012-01-19 Alkem Laboratories Ltd. Composition d'édulcorant et son procédé de production
AU2011338674B2 (en) * 2010-12-06 2017-03-30 Effrx Pharmaceuticals Sa Stable effervescent bisphosphonate formulations with rapid solubilization characteristics
EP2785200B1 (fr) * 2011-11-28 2018-03-28 Tate & Lyle Ingredients Americas LLC Edulcorant de table à flaveur naturelle améliorée
JP6099870B2 (ja) 2012-01-06 2017-03-22 松谷化学工業株式会社 スクロースとd−プシコースを含む新規甘味料
CN112522039B (zh) * 2020-12-14 2021-12-24 广州立白企业集团有限公司 一种衣物增香珠组合物及其制备方法

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AU2005235983A1 (en) 2005-11-03
AR048438A1 (es) 2006-04-26
IL178245A0 (en) 2006-12-31
JP2007530038A (ja) 2007-11-01
RU2006137296A (ru) 2008-04-27
CN1934277A (zh) 2007-03-21
WO2005103304A1 (fr) 2005-11-03
EP1730316A1 (fr) 2006-12-13

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