WO2024256701A1 - Gels d'émulsion de pectine à sensation en bouche améliorée - Google Patents

Gels d'émulsion de pectine à sensation en bouche améliorée Download PDF

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Publication number
WO2024256701A1
WO2024256701A1 PCT/EP2024/066687 EP2024066687W WO2024256701A1 WO 2024256701 A1 WO2024256701 A1 WO 2024256701A1 EP 2024066687 W EP2024066687 W EP 2024066687W WO 2024256701 A1 WO2024256701 A1 WO 2024256701A1
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Prior art keywords
pectin
oil
emulsion
based emulsion
water
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English (en)
Inventor
Sarah MICHEL
Stephanie MARTY-TERRADE
Sophie GROULT
Laurence Sandoz
Pol SEGARRA I CALBET
Julen BASCARAN REINKING
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Societe des Produits Nestle SA
Nestle SA
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Societe des Produits Nestle SA
Nestle SA
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    • 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
    • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
    • A23L29/206—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
    • A23L29/231—Pectin; Derivatives thereof
    • 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
    • A23D7/00—Edible oil or fat compositions containing an aqueous phase, e.g. margarines
    • A23D7/005—Edible oil or fat compositions containing an aqueous phase, e.g. margarines characterised by ingredients other than fatty acid triglycerides
    • A23D7/0056—Spread compositions
    • 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
    • A23L23/00—Soups; Sauces; Preparation or treatment thereof
    • 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
    • A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
    • A23L27/60—Salad dressings; Mayonnaise; Ketchup
    • 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
    • A23L35/00—Foods or foodstuffs not provided for in groups A23L5/00 - A23L33/00; Preparation or treatment thereof
    • A23L35/10—Emulsified foodstuffs
    • 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
    • A23L35/00—Foods or foodstuffs not provided for in groups A23L5/00 - A23L33/00; Preparation or treatment thereof
    • A23L35/20—No-fat spreads

Definitions

  • Emulsions, emulgels are frequently used in food matrices to bring fat-like attributes such as mouthcoating and stickiness.
  • Emulsions often consist in proteins as hydrocolloids and are very hydrophilic and not surface active.
  • Chemically modified hydrocolloids such as cellulose, any by further example methyl- or ethylcellulose, are surface active and can lead to oleogel formation but they are not well perceived by consumers.
  • Current emulsions used in cooking processes also have a tendency to not hold their shape during cooking and do not have good mouthcoating properties. There is a clear need to develop new emulsions that not only have an improved cooking performance but that also have better mouthcoating and stickiness attributes.
  • pectin which is a natural ingredient derived from for example vegetables and fruits
  • a clean label food product with improved sensory aspects can be obtained without other existing emulsifiers such as ethyl- or methyl-cellulose, gum arabic and lecithin, which are often perceived as unfavorable by consumers.
  • the present invention provides a stable emulsion in which small oil droplets with the average size of less than 20 pm are uniformly dispersed and homogenized in a continuous aqueous phase.
  • This stable emulsion can be clearly distinguished from a gelled matrix in which much bigger oil droplets are simply entrapped.
  • Such gelled matrix generally requires other emulsifiers or addition of calcium ions to stabilize.
  • the present invention enables an emulsion which can maintain improved stability even without other emulsifier or addition of calcium ion.
  • Figure 4B Storage and loss modulus for 6% pectin system as a function of calcium concentration at 25 and 80°C.
  • Figure 5A Oil droplet measurement of emulgels formulated with 4% of pectin and 20% of sunflower oil before heat treatment.
  • Figure 5B Oil droplet measurement of emulgels formulated with 4% of pectin and 20% of sunflower oil after heating at 80°C.
  • Figure 6A Oil droplet measurement of emulgels formulated with 4% of pectin, 20% of sunflower oil and 20 mM of calcium salt before heat treatment.
  • Figure 6B Oil droplet measurement of emulgels formulated with 4% of pectin, 20% of sunflower oil and 20 mM of calcium salt after heating at 80°C.
  • Figure 7A Oil droplet measurement of emulgels formulated with 6% of pectin and 20% of sunflower oil before heat treatment.
  • Figure 7B Oil droplet measurement of emulgels formulated with 6% of pectin, 20% of sunflower oil and 20 mM of calcium salt before heat treatment.
  • Figure 8 Storage modulus of emulsion gels with increasing concentrations of unsaturated Palm Stearin, as temperature is ramped from 25°C to 80°C.
  • Figure 13 Loss factor of emulsion gel containing 4% pectin, 20% high oleic sunflower oil, and additional fibers and starches.
  • Figures 18A Storage and loss modulus for samples stored at 4°C by the rheological method modulating the frequency in Example 11.
  • Figure 18B Storage and loss modulus for samples stored at 20°C by the rheological method modulating the frequency in Example 11.
  • Figure 19B Storage and loss modulus for samples stored at 20°C by the rheological method modulating the amplitude in Example 11.
  • FIG. 20A Viscosity for samples stored at 4°C in Example 11.
  • FIG. 20B Viscosity for samples stored at 20°C in Example 11.
  • Figure 21A Texture analysis results of carrot emulgels stored at 4°C in Example 11: hardness (positive force) and tack force (negative force).
  • Figure 21B Texture analysis results of carrot emulgels stored at 4°C in Example 11: positive and negative areas.
  • Figure 22A Texture analysis results of carrot emulgels stored at 20°C in Example 11: hardness (positive force) and tack force (negative force).
  • Figure 22B Texture analysis results of carrot emulgels stored at 20°C in Example 11: positive and negative areas.
  • FIG. 23B Tribology measurements of carrot emulgels stored at 20°C in Example 11.
  • Figure 24 Oil binding capacity of carrot emulgels stored at 4°C and at 20°C in Example 11.
  • Figure 25 Oil oxidation of carrot emulgels stored at 4°C and at 20°C in Example 11.
  • Figure 26 Oil droplet measurement of carrot emulgels of example 11 after heat treatment.
  • Figure 27A Oil droplet measurement of carrot emulgels of example 11 after 2 months of storage at 4°C.
  • Figure 27B Oil droplet measurement of carrot emulgels of example 11 after 6 months of storage at 4°C.
  • Figure 28A Oil droplet measurement of carrot emulgels of example 11 after 2 months of storage at room temperature.
  • Figure 28B Oil droplet measurement of carrot emulgels of example 11 after 6 months of storage at room temperature.
  • Figure 29A Texture attributes of recipes R1 to R5 as described in example 12.
  • Figure 29B Texture attributes of recipes R1 and R6 to R8 as described in example 12.
  • FIG. 30A Sensory attributes of recipes R1 to R5 as described in example 12.
  • FIG. 30B Sensory attributes of recipes R6 to R8 as described in example 12.
  • Figure 34 Acidity ranking of pectin emulgels as described in example 16.
  • the invention relates in general to pectin based emulsions.
  • the invention relates to a pectin based emulsion comprising pectin, oil, and water, wherein the emulsion has a pH which is less than 5.
  • the invention relates to a pectin based emulsion comprising pectin, oil, and water, wherein the emulsion has a pH which is less than the pKa of the pectin.
  • the invention relates to a pectin based emulsion comprising between 0.5 and 6 wt% pectin, oil, and water, wherein the emulsion has a pH which is less than 5.
  • the invention relates to a pectin based emulsion comprising pectin, between 3 and 40 wt% oil, and water, wherein the emulsion has a pH which is less than 5.
  • the invention relates to a pectin based emulsion comprising between 0.5 and 6 wt% pectin, between 3 and 40 wt% oil, and water, wherein the emulsion has a pH which is less than 5, an average oil droplet size in the emulsion is below 20 pm, and the pectin is high methoxy pectin with degree of methoxy (DM) > 60.
  • the emulsion has a pH which is less than 4.5, or less than 4.2, or less than 4, or about 3.5.
  • the average oil droplet size in the emulsion is below 19 pm, or below 18 pm, or below 17 pm, or below 16 pm, or below 15 pm.
  • the pectin is high methoxy pectin with degree of methoxy (DM) of 70.
  • the emulsion comprises multivalent ions.
  • the multivalent ions comprise calcium, magnesium or iron.
  • the multivalent ions are preferably calcium ions.
  • the emulsion comprises up to 80 mM multivalent ions.
  • the emulsion comprises between 5 and 40 mM multivalent ions.
  • said emulsion comprises about 2 wt% pectin and about 15 wt% oil.
  • the pectin is purified or non-purified.
  • the non-purified pectin is unrefined citrus fiber.
  • said emulsion further comprising fruit powder, vegetable powder, for example pulse flour, purified fibers, or purified starch.
  • the water is de-ionized water, tap water, or mineral water.
  • the water is replaced by a cooked puree, for example a vegetable puree, or a fruit puree, or a pulse puree.
  • a cooked puree for example a vegetable puree, or a fruit puree, or a pulse puree.
  • the pectin is a citrus pectin, a sugar beet pectin, an apple pectin, or an amidated pectin.
  • the invention further relates to a method of making a pectin based emulsion, said method comprising: heating between 0.5 and 6 wt% pectin in water to at least 50°C to obtain a hydrated pectin solution, adding between 3 and 40 wt% oil to the hydrated pectin solution; and mixing the mixture of the hydrated pectin solution and the oil by high shear mixing for about 5 minutes, wherein the emulsion has a pH which is less than 5, an average oil droplet size in the emulsion is below 20 pm, and the pectin is high methoxy pectin with degree of methoxy (DM) > 60.
  • DM methoxy pectin with degree of methoxy
  • the high shear mixing is performed while heating the mixture to at least 50°C, preferably about 75°C.
  • the high shear mixing is performed at a shear rate of between 170 and 3400 s-1. This shear rate corresponds to a rotational speed between 100 and 2000 RPM.
  • the method further comprises adjusting pH of the pectin based emulsion to be less than pH 5, preferably less than pH 4.5, more preferably less than pH 4.2, more preferably less than pH 3.5.
  • the pH is adjusted to about pH 3.5.
  • the method further comprises adding multivalent ions, preferably calcium ions to the pectin based emulsion after the high shear mixing.
  • multivalent ions are added to the pectin based emulsion after the high shear mixing, so that the final concentration of the multivalent ions in the pectin based emulsion reaches up to 80 mM, preferably between 5 and 40 mM.
  • the oil in the step of mixing the mixture of the hydrated pectin solution and the oil by high shear mixing, the oil is added at a constant flow of about 100 ml per minute.
  • the invention further relates to the use of a pectin based emulsion according to the invention, wherein said emulsion is a. a binder; b. a filling; c. a flavor carrier; d. a fat replacer; e. a spreadable product; f. a puree; g. a dip; h. a topping; or i. a frozen dessert.
  • said emulsion is a. a binder; b. a filling; c. a flavor carrier; d. a fat replacer; e. a spreadable product; f. a puree; g. a dip; h. a topping; or i. a frozen dessert.
  • the pectin based emulsion may comprise about 0.5 wt%, or about 1 wt%, or about 1.5 wt%, or about 2 wt% pectin, or about 3 wt% pectin, or about 4 wt% pectin, or about 5 wt% pectin, or about 6 wt% pectin, or about 7 wt% pectin, or about 8 wt% pectin, or about 9 wt% pectin, or about 10 wt% pectin.
  • the pectin based emulsion comprises about 2 wt% pectin or about 4 wt% pectin.
  • the starch may be a waxy corn starch.
  • the starch may be a potato starch.
  • the fat or oil may comprise animal fat or oil, vegetable fat or oil, for example a coconut oil or fat, sunflower oil and milk fat.
  • the oil may be sunflower oil, for example high oleic sunflower oil.
  • the pectin based emulsion may comprise palm stearin oil.
  • the pectin based emulsion may comprise about 3 wt%, or about 5 wt%, or about 10 wt%, or about 15 wt%, or about 20 wt%, or about 30 wt%, or about 40 wt%, or about 50 wt% oil.
  • the pectin based emulsion may comprise multivalent ions, for example magnesium, iron, or calcium ions, preferably calcium chloride dihydrate.
  • the pectin based emulsion may comprise about 1% calcium chloride dihydrate.
  • the pectin based emulsion may comprise about 5mM, or about 6mM, or about 7mM, or about 8mM, or about 9mM, or about lOmM, or about llmM, or about 12mM, or about 13mM, or about 14mM, or about 15mM, or about 16mM, or about 17mM, or about 18mM, or about 19mM, or about 20mM calcium chloride.
  • the pectin based emulsion comprises between 5 and 40 mM multivalent ions.
  • the multivalent ions for example calcium ions may be added to the pectin based emulsion after mixing and emulsifying the oil with the pectin solution for example by high shear mixing.
  • multivalent ions preferably calcium ions are added to the pectin based emulsion after mixing and emulsifying the oil with the pectin solution so that the final concentration of multivalent ions in the pectin based emulsion reaches up to 80mM, preferably between 5 and 40 mM.
  • the vegetable and/or fruit puree When vegetable and/or fruit puree is used as an aqueous phase to replace at least part of water in the pectin based emulsion, the vegetable and/or fruit puree may comprise some multivalent ions, for example magnesium, iron or calcium ions, and at least part of the final concentration of the multivalent ions in the pectin based emulsion may originate from the vegetable and/or fruit puree.
  • some multivalent ions for example magnesium, iron or calcium ions
  • the content of calcium ions in the vegetable and/or fruit puree may be on average between 10 and 40 mg per 100 g, or between 0.2 and 0.8 mmol per 100 g.
  • pectin based emulsion ingredients may comprise about 50 wt% water, about 60 wt% water, about 70 wt% water, about 80 wt% water, about 90 wt% water, or between 50 to 90 wt% water.
  • De-ionized water was found to provide a viscoelastic fluid. It was found to be useful for controlling melting properties.
  • the use of mineral water provides a gel-like material. Mineral water can be used as a source of calcium.
  • the pectin based emulsion may comprise potato starch, for example about 3wt% potato starch.
  • the pectin based emulsion may comprise waxy maize starch, for example about 3wt% waxy maize starch.
  • the pectin based emulsion may comprise wheat fiber, for example about 3wt% wheat fiber, or about 6wt% wheat fiber.
  • Preferred starches are waxy starch or potato starch. Starch was found to improve binding properties in both hot and cold applications. Potato starch was found to provide very good sensory attributes.
  • the pectin based emulsion may comprise pulse flour, preferably micronized pulse flour. Micronizing the flour was found to avoid graininess due to agglomeration.
  • the pectin based emulsion may, for example, comprise about 1.5-2.0 wt% pectin and about 10-15 wt% oil.
  • the pectin based emulsion may, for example, comprise about 4 wt% pectin and about 20 wt% oil.
  • the pectin based emulsion may, for example, comprise about 4 wt% pectin and 20 wt% oil in deionized water.
  • the pectin based emulsion has a pH less than 5, preferably less than 4.5, preferably less than 4.2, preferably less than 4, preferably less than 3.5.
  • the pH may be about pH 2.
  • the pectin based emulsion may comprise about 3wt% pectin, about 8wt% soy flour and about 20wt% fat.
  • the pectin based emulsion may comprise about 8wt% pectin, and about 10wt% fat.
  • the pectin based emulsion may comprise about 4wt% pectin, and about 40wt% fat.
  • the food product comprising the pectin based emulsion may be a vegetable puree spread.
  • the puree may comprise red bell pepper puree, carrot puree, or broccoli puree.
  • the food product may have a recipe substantially similar to that shown in table 16.
  • the food product may be a spreadable liquid like matrix, wherein the product comprises an emulsion with about 2wt% pectin and about 15wt% oil.
  • the pectin based emulsion may be used as a flavor enhancer.
  • the flavor enhancer may have a recipe substantially similar to that shown in table 19 (R8).
  • the pectin based emulsion may be used as a puree, for example as a baby food puree.
  • the example of baby food puree may comprise about between 0.5 and 1.5 wt% pectin and about between 3 and 7 wt% fat or oil.
  • the pectin based emulsion may be used as an ice cream, gelato or frozen dessert.
  • the example of frozen dessert may comprise about between 1 and 2 wt% pectin, about between 3 and 20 wt% fat or oil, and about between 60 and 95 wt% vegetable and/or fruit purees.
  • the example of frozen dessert may further comprise sugar.
  • the pectin can be hydrated with water.
  • the water may be mineral water, for example Vittel water.
  • the water may be tap water.
  • the water may be deionized water.
  • the pectin can also be hydrated with water contained in vegetable and/or fruit puree.
  • the hydration step may last for about 15 min, and be done at about 50 °C.
  • a pasteurization step may be done for about 5 min at about 75 °C. Both may be performed at about speed 2.5 in a Thermomix (350 RPM).
  • the pasteurization step may optionally be performed only for the purpose of safety for consumption, and the pectin based emulsion according to the present invention is stable without such optional pasteurization step.
  • oil is added to the pectin solution, and the pectin solution can be emulsified for about 5 minutes, for example by high shear mixing.
  • the high shear mixing may be performed while heating the mixture to at least 50°C, preferably about 75°C.
  • the high shear mixing may be performed at a shear rate of between 170 and 3400 s-1, which corresponds to a rotational speed between 100 and 2000 RPM.
  • the shear speed of the Thermomix may be increased to about 4.5 (1550 RPM) and the oil added in a constant flow of about 100 ml per minute.
  • calcium chloride may be added during the last minute of emulsification, or after the emulsification.
  • the method may further comprise a step of retorting the pectin based emulsion.
  • the retorting step may be performed at 95°C for 5 min.
  • the pectin based emulsion may be used as (i) a binder, for example which holds upon cooking so the product can be flipped on the pan while cooking.
  • the emulsion comprises calcium and starch; (ii) a filling, for example inside a matrix so the emulsion thins upon cooking but without phase separation (for example, croquette and burrata); (iii) a flavor carrier, for example by incorporating spices inside a food matrix; (iv) a fat replacer, for example where the emulsion destabilizes during cooking and enhances the juiciness in the final food product; (v) spreadable product; (vi) a puree; (vii) a dip; (viii) a topping; or (ix) a frozen dessert.
  • the singular forms "a,” “an” and “the” include plural referents unless the context clearly dictates otherwise.
  • compositions disclosed herein may lack any element that is not specifically disclosed.
  • a disclosure of an embodiment using the term “comprising” includes a disclosure of embodiments “consisting essentially of and “consisting of the components identified.
  • the methods disclosed herein may lack any step that is not specifically disclosed herein.
  • a disclosure of an embodiment using the term “comprising” includes a disclosure of embodiments “consisting essentially of” and “consisting of” the steps identified.
  • a vegan product is defined as being devoid of animal products, for example devoid of dairy products and meat products.
  • a vegan analogue product of the invention has the look, taste, and texture which is close to real animal based product.
  • the first step of producing the emulgels was hydration of the pectin with water (Vittel or tap or deionized) for 15 min at 50 °C, and a pasteurisation step of 5 min at 75 °C in order to make the gels safe for consumption. Both were performed at speed 350 RPM.
  • the pectin solution was emulsified for 5 minutes by high shear mixing . During the high shear mixing, the shear speed was increased from 350 RPM to 1550 RPM, and the oil was added in a constant flow of 100 mL per minute.
  • CaCL was added during the last minute of emulsification.
  • Solid-like samples stainless-steel parallel plate geometry of 50 mm of diameter and serrated surface (PP50/SS/P2) to prevent a slippery effect with a gap distance of 1 mm.
  • PP50/SS/P2 stainless-steel parallel plate geometry of 50 mm of diameter and serrated surface
  • Samples were loaded at 4°C and were heated to 90°C (5°C/min, 0.2% strain, 1 Hz), cooked at 90°C for 1 min and cooled down to 60°C (5°C/min, 0.2% strain, 1 Hz ; holding time 3 min) then to 40°C (5°C/min, 0.2% strain, 1 Hz ; holding time 3 min).
  • Frequency sweeps (0.02% y, 0.01-10 Hz) were performed at 4°C and after cooling at 40°C.
  • the storage modulus G', the loss modulus G" and the loss factor tan delta were recorded at 4°C, 40°C in the heating step, 90°C and 40°C in the cooling step.
  • Possible routes to produce a gel with the desired properties were identified: (i) TA, high tack force and work of adhesiveness High pectin level, coupled with low oil level; (ii) [Rheology] High G' and low tan delta at 40°C cooling High oil level, coupled with calcium addition; and (iii) [Rheology] High G' and low tan delta at 90°C High oil level, coupled with calcium addition.
  • Table 1 shows impact on increasing the content of the formulation parameters (pectin, oil and calcium) on the emulsion-gel properties and the R 2 values of the linear model regressions for each analytical parameter. Arrows pointing down mean a decrease on that parameter and pointing up an increase. The type and number of arrows indicates the level of significance.
  • the samples were tasted at the ambient temperature (25°C) or in a heated state (60°C), and assessed by a trained panel using a rate all that apply methodology consisting in first listing all the attributes related to the sample, and then rate these attributes from 1 (slightly intense) to 5 (strongly intense).
  • the sensory glossary used is given in Table 5.
  • demineralized water was shown to strongly increase the slipperiness and melting, while decreasing the oil leaking, firmness, stickiness and mouthcoating. Therefore, filling formulations should favor the use of demineralized water, when the presence of minerals favour heatstability and are better suited for binding applications.
  • the gel exhibits more liquid state behavior as the loss modulus was greater than the storage. This manifests as a much less viscous fluid like emulsion, rather than a more solid like gel seen at higher additions of calcium.
  • lOmM calcium solution Upon addition of lOmM calcium solution, a dramatic increase in solid like behavior is observed, as the storage modulus increases by greater than a factor of three from 91 Pa to 289 Pa in the 4% mixture.
  • the rheological results demonstrate a storage modulus greater than the loss, now indicating that the gel exhibits a more solid like behavior.
  • the pectin based emulsion according to the present invention provides a fluid-like emulsion in which small oil droplets with the average size of less than 20 pm are well dispersed and homogenized in the continuous aqueous phase.
  • the emulsion according to the present invention enables improved stability, versatility for e.g. liquid or fluid applications, as well as more controllable texture.
  • the present invention provides such stable and homogenous emulsion even without calcium addition.
  • the high methoxy pectin derived from citrus used was replaced by: a low methoxy pectin derived from citrus, an apple pectin, a sugar beet pectin, an amidated pectin derived from citrus, and an unrefined citrus fiber.
  • the citrus fiber may be considered as non-purified pectin compared to the purified high methoxy pectin derived from citrus.
  • the emulsion was generated from 4% pectin and 20% oil in MQ. water.
  • the emulgels were heated up to 90°C and cooled down to 40°C to assess the stability.
  • High methoxy and sugar beet pectin emulgels have a strong liquid-like behaviour (tan delta > 1) whereas citrus fiber or low methoxy pectins are gels. All materials thinned with cooking (increase in tan delta) but the sugar beet formulation was the least affected of all.
  • Using a pectin-rich citrus fiber (40% pectin) allowed strongly improved the gel-like character and the heat stability. This suggests the emulgel properties and heat resistance can be tuned by modifying the pectin structure and degree of methoxylation in addition to the calcium content. None of the emulgel phase separated with heating but the apple pectin ones turned very thin.
  • Palm stearin contains up to 50% palmitic acid, a fully saturated fatty acid which allows for the oil to retain a solid form at room temperature. This contrasts with the high oleic sunflower oil, which is comprised almost entirely of unsaturated oleic acid and exists as a liquid at room temperature.
  • the oil mixtures were heated to 55°C, well above the melting point of palm stearin. The oils were then incorporated under high shear in an identical fashion to the gels containing only high oleic sunflower oil.
  • the storage modulus (G') is selected for plotting as it represents the solid behavior of the gel. Notable is the different storage modulus values at room temperature as the amount of saturated oil is increased in the gel matrix. As the temperature is fixed at 25°C, the lowest G' values are observed for the 0, and 25% additions of palm stearin to high oleic oil. At values greater than 25% addition, a trend is observed where the more saturated fat added, the greater the G' value, with the 100% palm stearin gel displaying a dramatically higher G' value at 25°C.
  • the solid nature of the fat was found to lend rigidity to the gel matrix at temperatures below the melting point. As the temperature is ramped to 80°C the solid fat begins to melt, which manifests as a drop in the G' values. At the 80°C final temperature the inverse trend is seen. Gels containing higher amounts of saturated fats display lower G' values.
  • Figure 9 illustrates the results of the probe tack test and the visual appearance of the samples.
  • Samples Pl and P2 differ in dissolution time to hydrate the pectin, for Pl dissolution was at 50 °C during 15 min with Vittel water, and for P2 dissolution was at 50 °C during 2 h with Vittel water. Although there were no visual differences in the gels, sample P2 exhibited significantly higher adhesiveness (1.617 ⁇ 0.27 N*s) compared to Pl (1.10 ⁇ 0.14 N*s), which had a shorter solubilization time, while the tack force remained similar.
  • the higher oil binding capacity observed in this study could be attributed to the increased polymer extension of the pectin chains, which is a result of the longer hydration time.
  • the extended polymer chains may expose methyl groups that could be previously confined within the pectin structure, creating chain configurations that can be described as "hydrophobic pockets.” With a longer solubilization time, these pockets are displaced and become available to interact with the oil droplets. The intensified interaction between the exposed hydrophobic pockets and the oil droplets leads to enhanced binding and stabilization within the gel structure.
  • Figure 13 shows the loss factor of a 4% pectin, 20% oil emulsion gel with varying fibers and starches. Addition of these fibers has a notable effect on the rigidity of the gel as seen by the drop in loss factor at room temperature.
  • Potato starch showed the least significant decrease, followed by wheat fiber. Waxy maize starch showed the most significant decrease in loss factor at both low and high temperatures. Additionally, from the wheat fiber additions, it is seen that increasing the amount of fiber decreases the loss factor further.
  • starches and fibers also affect the texture of the emulsion gels. Addition of these fibers have notable impacts on the hardness, tack force, and work of adhesion. Seen in table 10, the addition of starch and fiber results in similar trends seen in the rheological results. Potato starch shows the smallest change, followed by the wheat fiber, and the waxy maize. These results indicate that addition of fibers and starches can increase the stickiness of the gels, and can lead to overall much firmer textures.
  • Table 10 Texture analysis values for emulsion gels containing added fibers and starches.
  • a soy protein gel was prepared by hydrating 20% of soy protein in water for 15 min.
  • the soy protein dough was placed on a plastic film to make a layer, then emulgel filling (whose recipe is disclosed in table 14) was added in the middle and the film was closed to make a small ball which was cooked in a steam oven. After cooking the ball could be open and cut through to let a liquid filling flow out.
  • the sample had the appearance of a burrata, with a liquid core entrapped in a solid shell. It could be heated without melting.
  • the recipe given for a filling in table 14 was placed in half-sphere silicon moulds and frozen overnight. The following days spheres were demolded and assembled to make a single sphere, which breaded with egg and breadings then deep fried. The croquettas could be successfully fried and presented a liquid core. Vegetable pieces could be included into the ball.
  • a binder was prepared as disclosed in table 14, then combined with the ingredients disclosed in table 15 to form a wet dough, which was shaped as a croquette and pan fried.
  • the croquetta could be pan fried and flipped over, while still maintaining its shape and without losing vegetable or TVP pieces, confirming the binding properties of pectin emulgels. It presented a very indulgent mouthfeel from the pectin, unlike the dry mouthfeel often felt for plant-based meat analogs.
  • Emulsion gels with high puree content were prepared as described earlier using puree instead of water.
  • the pH was adjusted to 4.2 with vinegar to ensure emulsion formulation, because vegetables with higher pH (higher than pH 5, for example) may not be efficiently emulsified and led to oil separation as reported in previous sections.
  • the spread was prepared as described in Example 10.
  • the amount of acid was increased to ensure food safety.
  • the emulsion was transferred to glass jars, sealed, and retorted in a steam oven so that the core temperature reached 95°C for 5 min.
  • the glass jars were stored either in a fridge at 4°C or at room temperature at 25°C over 6 months. The stability was assessed before and after heat treatment, after 2 weeks, 1 month, 1.5 month, 2 months, 3 months and 6 months. Stability of the gel was probed throughout the shelf life test with the following methods: rheological method modulating the frequency to monitor the storage and loss modulus for both the samples stored at 4°C, and the samples stored at 20°C (figures 18A and 18B). rheological method modulating the amplitude to monitor the storage and loss modulus for both the samples stored at 4°C, and the samples stored at 20°C (figures 19A and 19B).
  • the average oil droplet size for the samples stored at room temperature is still below 20 pm, even after 6 months.
  • the pectin based emulsion according to the present invention enables an emulsion which can maintain the good stability even after 6 months under the room temperature condition.
  • Pectin emulgels and impact on flavour and texture perception The sensory attributes of acidified pectin emulgels were assessed on the following recipes in Table 19.
  • Pectin addition reduced the overall flavour perception, including the bitterness induced by lactic acid and the vegetable flavour.
  • Emulgel samples (R5) were perceived slightly less acidic than acidified puree, but the differences were not significant, (figure 30A).
  • the addition of pectin in curry-flavoured puree (R7) increased the spiciness perception but also the bitterness, whereas pectin emulgels were significantly less bitter while maintaining a strong curry flavour (figure 30B).
  • a grouping of all products showed that pectin samples were not described as acidic unlike acidified purees (figure 31). This demonstrates the benefit of pectin emulgels in masking off-flavours.
  • Pectin emulgels could also be formulated using fruit purees. Example recipes are described in Table 21. The emulgels were prepared as described in the previous examples and were successively frozen. Frozen desserts were freshly prepared using a Pacojet. The pectin used in this example was a high methoxy pectin from citrus with a degree of methoxylation around 70%.
  • Recipe D was shiny and perceived as fruity and fatty, rich, hearty.
  • Recipe E was very aerated and hearty. It could be used as a coating.
  • Baby purees were prepared from pectin emulgels to improve stability and texture.
  • the pectin used in this example was a high methoxy pectin from citrus with a degree of methoxylation around 70%.
  • To adapt the texture to indulgent purees low pectin concentrations were preferred in formulations.
  • the recipes are summarized in table 22.
  • the emulgels were prepared as described earlier, then the samples were heated to 90°C for 5 min and filled in a glass jar which was closed and inverted for 90 sec to ensure shelf stability.
  • the samples were assessed for 2 weeks following heat treatment in terms of colour and viscosity.
  • Table 23 Colour variation of emulgel purees after heat treatment (HT)
  • the reference carrot puree clearly formed 2 phases after heat treatment, whereas the emulgel purees remained homogeneous.
  • the viscosity decreased slightly and remained stable over 3 weeks. This demonstrates the superiority of emulgel purees for the stability of baby food purees.
  • Cooking sauces were prepared according to the recipe disclosed in table 25.
  • the products obtained with these recipes had a lower viscosity than the dips given in example 10.
  • the products were less sticky and mouthcoating.
  • the mouthfeel was rich and indulgent and the spices were long perceived in mouth.
  • the texture and viscosity was close to that of a barbecue sauce or a ketchup.
  • the pectin was hydrated at room temperature (25°C) then a solution of CaCL IM was added to reach a final concentration of 5 mM; finally, the emulsification was performed at 25°C.
  • the pectin was hydrated at 50°C and the emulsification was performed at 75°C; the CaCL solution was added after the emulsification was performed.
  • Samples Cl and C2 presented different viscoelastic properties, as seen in Figure 32.
  • Cold emulsified samples (Cl) had a weak gel-like behavior while C2 behaved like a viscoelastic fluid. Such a big difference in rheological properties was not expected by a simple variation in emulsification temperature.
  • the oil droplet size was compared for both samples. While hot emulsification samples (C2) provided oil droplet sizes below 20 pm, the samples with emulsification at 25°C (Cl) provided bigger oil droplet dimensions of about 25 pm ( Figures 33A and 33B). Hot emulsification allows for lower viscosity of the pectin continuous phase and for the oil phase, which will be easier to disperse under shearing, resulting in smaller oil droplets which have a significant impact on the material properties.
  • Sample DOI was the most acidic (score 7.1) while both emulgels samples were significantly less acidic (score 4.4 for D02 and 2.1 for D03). D03 was significantly less acidic than D02.

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Abstract

La présente invention concerne une émulsion à base de pectine, ladite émulsion comprenant entre 0,5 et 6 % en poids de pectine, 3 et 40 % en poids d'huile, et de l'eau, l'émulsion ayant un pH qui est inférieur à 5, une taille moyenne de gouttelettes d'huile dans l'émulsion étant inférieure à 20 pm, et la pectine étant une pectine à teneur élevée en méthoxy avec un degré de méthoxy (DM) > 60.
PCT/EP2024/066687 2023-06-16 2024-06-14 Gels d'émulsion de pectine à sensation en bouche améliorée Pending WO2024256701A1 (fr)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0426434A1 (fr) * 1989-11-01 1991-05-08 The Western Sugar Company Pectines de betteraves à sucre et leur utilisation pour des produits comestibles
US20050048181A1 (en) * 2002-05-16 2005-03-03 Jean-Luc Gelin Flavored oil-in-water emulsions for food applications
WO2014001030A1 (fr) * 2012-06-27 2014-01-03 Unilever N.V. Émulsion huile dans eau comestible
CN112056544A (zh) * 2020-09-21 2020-12-11 华中农业大学 一种可稳定负载脂溶性活性成分的果胶乳液凝胶的制备方法
CN113475707A (zh) * 2021-07-13 2021-10-08 江西莱檬生物科技有限责任公司 一种基于果胶的乳液凝胶及其制备方法与应用
WO2022266588A1 (fr) * 2021-06-15 2022-12-22 Whitewave Services, Inc. Compositions de pectine de betterave

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0426434A1 (fr) * 1989-11-01 1991-05-08 The Western Sugar Company Pectines de betteraves à sucre et leur utilisation pour des produits comestibles
US20050048181A1 (en) * 2002-05-16 2005-03-03 Jean-Luc Gelin Flavored oil-in-water emulsions for food applications
WO2014001030A1 (fr) * 2012-06-27 2014-01-03 Unilever N.V. Émulsion huile dans eau comestible
CN112056544A (zh) * 2020-09-21 2020-12-11 华中农业大学 一种可稳定负载脂溶性活性成分的果胶乳液凝胶的制备方法
WO2022266588A1 (fr) * 2021-06-15 2022-12-22 Whitewave Services, Inc. Compositions de pectine de betterave
CN113475707A (zh) * 2021-07-13 2021-10-08 江西莱檬生物科技有限责任公司 一种基于果胶的乳液凝胶及其制备方法与应用

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Title
DU LE HOANG ET AL: "Pectin emulsions for colon-targeted release of propionic acid", FOOD HYDROCOLLOIDS, ELSEVIER BV, NL, vol. 103, 25 December 2019 (2019-12-25), XP086077394, ISSN: 0268-005X, [retrieved on 20191225], DOI: 10.1016/J.FOODHYD.2019.105623 *

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