WO2018018112A1 - Procédé pour l'obtention de germes de cristallisation, germes de cristallisation et leurs utilisations - Google Patents
Procédé pour l'obtention de germes de cristallisation, germes de cristallisation et leurs utilisations Download PDFInfo
- Publication number
- WO2018018112A1 WO2018018112A1 PCT/BR2017/000084 BR2017000084W WO2018018112A1 WO 2018018112 A1 WO2018018112 A1 WO 2018018112A1 BR 2017000084 W BR2017000084 W BR 2017000084W WO 2018018112 A1 WO2018018112 A1 WO 2018018112A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- crystallization
- seeds
- crystallization seeds
- temperature
- limonene
- 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.)
- Ceased
Links
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS OR COOKING OILS
- A23D9/00—Other edible oils or fats, e.g. shortenings or cooking oils
- A23D9/02—Other edible oils or fats, e.g. shortenings or cooking oils characterised by the production or working-up
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23G—COCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF
- A23G1/00—Cocoa; Cocoa products, e.g. chocolate; Substitutes therefor
- A23G1/30—Cocoa products, e.g. chocolate; Substitutes therefor
- A23G1/32—Cocoa products, e.g. chocolate; Substitutes therefor characterised by the composition containing organic or inorganic compounds
- A23G1/36—Cocoa products, e.g. chocolate; Substitutes therefor characterised by the composition containing organic or inorganic compounds characterised by the fats used
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K20/00—Accessory food factors for animal feeding-stuffs
- A23K20/10—Organic substances
- A23K20/158—Fatty acids; Fats; Products containing oils or fats
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/115—Fatty acids or derivatives thereof; Fats or oils
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/44—Oils, fats or waxes according to two or more groups of A61K47/02-A61K47/42; Natural or modified natural oils, fats or waxes, e.g. castor oil, polyethoxylated castor oil, montan wax, lignite, shellac, rosin, beeswax or lanolin
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/92—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
Definitions
- the present invention is in the food and beverage field and relates to a process for obtaining crystallization seeds using mixtures of ihardfat fully hydrogenated soybean oil), potential for accelerating and modifying crystallization of Fats such as crystallization seeds in polymorphic forms are most useful.
- Cocoa butter is the major component in chocolates, characterizing the product's continuous phase as a dispersing matrix for solid cocoa, sugar and milk particles (LOISEL et al., 1998).
- This fat can crystallize into 6 polymorphic forms, each with distinct thermodynamic stability and melting point, identified as X, II, III, IV, V and VI, or by Greek letters, y,, ⁇ 'and ⁇ . the most stable form VI (WILLE & LU TON, 1966).
- the V or ⁇ form is the most desirable polymorph for chocolate (HINDLE, POVEY and SMITH, 2002).
- the tempering process of chocolate is fundamentally a controlled crystallization in which, through heat and mechanical treatments, a specific percentage of crystals is produced in the most stable form of MC (HARTEL, 1991). Effective tempering can facilitate demolding, prevent fat-bloom from cooling and storage, and obtain a finished product with good gloss, texture (snap) and fusion characteristics.
- TAGs active triglyceride nucleating agents
- PPP tripalmitin
- POP 1-palmityl-2-ooyoyl palmitin
- SOS 1-stearyl-2-oleoylstearine
- Lopes et al. (2015) developed spray cooling crystallization seeds employing soybean, cotton, palm and crambe hardfats, fully hydrogenated vegetable oils, which have a homogeneous high melting TAG composition.
- Hardfats represent low cost industrial fats with great potential for modification and acceleration of cocoa butter crystallization (RIBEIRO et al. 2Q13).
- Lipid microparticles (SLM) or soybean hardfat crystallization seeds obtained by Lopes et al. (2015) demonstrated the need for storage under controlled temperatures (between 25 and 45 ° C) for 1 to .139 days, aiming at the transition from unstable polymorphic forms ( ⁇ ) obtained after particle production to stable forces ( ⁇ ). Storage at 45 ° C for 24 hours allowed the transition to the ⁇ form.
- high temperatures favored the agglomeration of SIM,
- the present invention relates the use of the D-Lemonene polymorphic transition acceleration potential, verified in static crystallization of MC, for the production of stabilized crystallization seeds (form 3), which demonstrates the unprecedentedness. of the idea.
- the idea is not just a simple application of D-limonene on a different lipid basis, but the production of stabilized microparticles by means of this monomer.
- the present invention relates the use of the D-Limenon polymorphic transition acceleration potential, found in static crystallization of MC, to the production of stabilized crystallization seeds ( ⁇ form), which demonstrates the novelty of the idea.
- the idea is not just a simple application of D-limonene on a different lipid basis, but the production of stabilized microparticles through this raonoterpene, aiming at application in chocolates and other industrial products or processes.
- the chocolate therapy step is the formation of crystallization nuclei of the lipid phase of chocolate, with the formation of approximately 4% of stable beta-type crystals by a specific heat treatment. These crystals of triacylglycerol nature are responsible for structuring the crystal lattice in this stable form (beta), which characterizes the quality chocolate.
- the present invention aims to propose a process for obtaining crystallization seeds under the stable ⁇ polymorphic habit, composed of mixtures between fully hydrogenated soybean hardfat oil and different concentrations of D-limonene or soybean oil. canola, obtained by spray cooling technique.
- PMF medium palm fraction
- FIG. IA shows the micrograph of pure soybean hardfat seeds performed at 25 ° C at 150x magnification, 500 bar;
- FIG. 1B shows micrograph of soybean hardfat seeds with the addition of 5% D-limonene performed at 25 ° C in 150x magnification, 500u bar;
- FIG. 1C shows micrograph of hardfat seeds with 7.5% canola oil addition performed at 25 ° C in 150x magnification, SOOpra bar;
- FIG. 2A shows the XRD pattern (short spacing) of soybean hardfat microparticles, at times 0, 2, 7, 19 and 26 days at 25 ° C without addition of oils;
- FIG. 2B shows the short spacing of the soybean hardfat microparticles at times 0, 4, 7, 19 and 26: days at 25 ° C with. addition of 7.5% canola oil;
- FIG. 2C shows ⁇ diffractogram (short spacing) of the soybean hardfat microparticles at times 0, 2, 7, 1.9 and 26 days at 25 ° C with 5% D-limonene added.
- FIG. 3 shows the tempering curve obtained for milk chocolate, with and without the addition of the microparticles of the invention: (a) conventional sealing, (b) tempering with addition of soybean hardfat + canola oil microparticles and (c) tempering with the addition of soybean hardfat art D-lirnonene microparticles,
- the present invention relates to a process for obtaining crystallization seeds under the more stable polymorphic habit ⁇ ' , composed of mixtures between soybean hardfat and different concentrations of D-i.monene or canola oil comprising the following steps-- a) melt the hardfat. soybeans, for example in a bath, hot tanks or in a microwave oven, at a temperature ranging from 70 to 90 ° C, preferably from 75 to 80 ° C until complete melting of the fat crystals;
- jacketed medium mixture for example in jacketed tank, under controlled temperature of L 70 to 90 C for 6 minutes;
- atomizing the mixture was spray cooling system which may comprise a container maintained at -10 ° to 1.0 ° C, preferably between -2 and the 0 ° C using nozzle atora 0.2 to Zador 2 mm, preferably from 0.7 to 1 liter and compressed air pressures varying from 0.5 to 5 kgf / cm 2 , preferably from 1.0 to 2.0 kgf / cm 2 at room temperature;
- g store in closed containers in a temperature controlled chamber of 10 to 30 ° C, preferably ⁇ 25 ° C.
- Crystallization seeds were produced by the method described above using the spray cooiing technique initially with the addition of 1 to 15% d-limonene or cinnamon oil to the hardfat. soybeans, resulting in a relatively loose powder with no agglomeration.
- Seed surfaces were evaluated by Scanning Electron Microscopy (ME). Water was used aluminum base (1.4 cm diameter by 0.6 thickness) with double sided copper tape and colloidal graphite layer. Then the seeds were pulverized and fixed in this structure, and the samples were analyzed under table type microscope with variable voltage acceleration of 10 kV, with 150 times increase.
- ME Scanning Electron Microscopy
- the crystallization seeds produced are visually presented as relatively loose powders without agglomeration. Scanning electron microscopy (MBV) showed its spherical shape and confirmed the absence of agglomeration. In addition, a smooth and homogeneous surface has been shown to prove the beneficial effect of D-limonene or canola oil on crystallization of hazdfat and on the formation of crystallization seeds.
- MBV scanning electron microscopy
- the mean diameter (D 5 a) of the microparticles was between 150 and 2,00pm, for comparison, the literature indicates a diameter of the microparticles range from 5 to 500 u for satisfactory application as crystallization seeds, Therefore, microparticles present this potential application.
- Polymorphic seed habit was determined by X-ray diffraction according to the AOCS Cj 2-95 method (AOCS, 2009). Was. used: a diffractometer using geometry. Bragg-Brentano ( ⁇ : 2 ⁇ ) with Cu- ⁇ radiation (k - 1.5418 ⁇ , 40KV voltage and 30mA current). Measurements were obtained with steps of 0.02 ° In 20 and acquisition time of 2s, with scans of 15 to 30 ° (2 ⁇ scale). The identification of the polymorphic form was determined from the values of the shorts spacings (distances between the parallel acyclic groups in the triacylglycerol) characteristic of the crystals.
- FIG. 2A shows the diffractograms of the oil-free soybean harclfat sample and FIG. 2B of the sample with 7.5% canola oil added and FIG. 2C with addition of 5% D-1 imonene.
- the crystallization seeds of the present invention under the most stable polymorphic habit B are composed of mixtures of soybean fully hydrogenated oil (kardfat) and different concentrations of D-limonene or canola oil obtained by Spray cooling technique features, the induction of crystals in the polyrriorphic form ⁇ , which is desirable in products such as chocolate due to the ability to accelerate or render unnecessary the expensive tempering or pre-crystallization stage.
- crystallization seeds of the present invention may be applied to food, cosmetic, pharmaceutical and veterinary products to accelerate crystallization in fat crystallization and oil structuring processes.
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Epidemiology (AREA)
- Animal Behavior & Ethology (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Inorganic Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- Pharmacology & Pharmacy (AREA)
- Nutrition Science (AREA)
- Medicinal Chemistry (AREA)
- Animal Husbandry (AREA)
- Zoology (AREA)
- Mycology (AREA)
- Birds (AREA)
- Confectionery (AREA)
- Edible Oils And Fats (AREA)
- Fats And Perfumes (AREA)
Abstract
La présente invention concerne un procédé pour l'obtention de germes de cristallisation potentielle dans l'accélération et la modification de la cristallisation de graisses, ainsi que des germes de cristallisation sous formes polymorphes plus stables (forme β).
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| BRBR1020160178690 | 2016-07-29 | ||
| BR102016017869-0A BR102016017869B1 (pt) | 2016-07-29 | 2016-07-29 | Processo para a obtenção de sementes de cristalização, sementes de cristalização e uso das mesmas |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| WO2018018112A1 true WO2018018112A1 (fr) | 2018-02-01 |
Family
ID=61015162
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/BR2017/000084 Ceased WO2018018112A1 (fr) | 2016-07-29 | 2017-07-28 | Procédé pour l'obtention de germes de cristallisation, germes de cristallisation et leurs utilisations |
Country Status (2)
| Country | Link |
|---|---|
| BR (1) | BR102016017869B1 (fr) |
| WO (1) | WO2018018112A1 (fr) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2785983A (en) * | 1953-06-23 | 1957-03-19 | Buckeye Cellulose Corp | Flavoring material and method of making the same |
| US3582353A (en) * | 1968-02-19 | 1971-06-01 | Campbell Taggart Ass Bakeries | Edible products with localized areas of coloring or flavoring and process for making same |
| US3949094A (en) * | 1974-07-31 | 1976-04-06 | Scm Corporation | Condiment-treating process and product |
| BR9802593A (pt) * | 1997-07-24 | 2000-11-28 | Nestle Sa | Chocolate com baixo teor de gordura |
| US6245366B1 (en) * | 1996-10-25 | 2001-06-12 | Mccormick & Company, Inc. | Fat-coated encapsulation compositions and method for preparing the same |
| WO2009058381A1 (fr) * | 2007-10-31 | 2009-05-07 | Swedish Match North America, Inc. | Procédé de fabrication de dispersions particulaires solides aromatisées |
| BR102012024791A2 (pt) * | 2012-09-17 | 2016-03-29 | Unicamp | processo para estabilização de manteiga de cacau e chocolate, processo para obtenção de sementes de cristalização, sementes de cristalização, produtos estabilizados e usos |
-
2016
- 2016-07-29 BR BR102016017869-0A patent/BR102016017869B1/pt active IP Right Grant
-
2017
- 2017-07-28 WO PCT/BR2017/000084 patent/WO2018018112A1/fr not_active Ceased
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2785983A (en) * | 1953-06-23 | 1957-03-19 | Buckeye Cellulose Corp | Flavoring material and method of making the same |
| US3582353A (en) * | 1968-02-19 | 1971-06-01 | Campbell Taggart Ass Bakeries | Edible products with localized areas of coloring or flavoring and process for making same |
| US3949094A (en) * | 1974-07-31 | 1976-04-06 | Scm Corporation | Condiment-treating process and product |
| US6245366B1 (en) * | 1996-10-25 | 2001-06-12 | Mccormick & Company, Inc. | Fat-coated encapsulation compositions and method for preparing the same |
| BR9802593A (pt) * | 1997-07-24 | 2000-11-28 | Nestle Sa | Chocolate com baixo teor de gordura |
| WO2009058381A1 (fr) * | 2007-10-31 | 2009-05-07 | Swedish Match North America, Inc. | Procédé de fabrication de dispersions particulaires solides aromatisées |
| BR102012024791A2 (pt) * | 2012-09-17 | 2016-03-29 | Unicamp | processo para estabilização de manteiga de cacau e chocolate, processo para obtenção de sementes de cristalização, sementes de cristalização, produtos estabilizados e usos |
Non-Patent Citations (5)
| Title |
|---|
| DEMAN, L. ET AL.: "Polymorphic behavior of some fully hydrogenated oils and their mixtures with liquid oil", JOURNAL OF THE AMERICAN OIL CHEMISTS' SOCIETY, vol. 66, no. 12, December 1989 (1989-12-01), pages 1777 - 1780, XP055460851 * |
| MIYASAKI, E.K. ET AL.: "Acceleration of polymorphic transition of cocoa butter and cocoa butter equivalent by addition of D-limonene", EUROPEAN JOURNAL OF LIPID SCIENCE AND TECHNOLOGY, vol. 118, no. 5, May 2016 (2016-05-01), pages 716 - 723, XP055460849 * |
| PEREZ-MARTINEZ, D. ET AL.: "The cooling rate effect on the microstructure and rheological properties of blends of cocoa butter with vegetable oils", FOOD RESEARCH INTERNATIONAL, vol. 40, no. 1, January 2007 (2007-01-01), pages 47 - 62, XP005764698 * |
| RAY, J. ET AL.: "The effect of limonene on the crystallization of cocoa butter", JOURNAL OF THE AMERICAN OIL CHEMISTS' SOCIETY, vol. 89, no. 3, March 2012 (2012-03-01), pages 437 - 445, XP035017486 * |
| RIGOLLE, A. ET AL.: "Isothermal crystallization behavior of cocoa butter at 17 and 20 °C with and without limonene", JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY, vol. 64, no. 17, April 2016 (2016-04-01), pages 3405 - 3416, XP055460848 * |
Also Published As
| Publication number | Publication date |
|---|---|
| BR102016017869B1 (pt) | 2022-04-12 |
| BR102016017869A2 (pt) | 2018-02-14 |
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