METHOD FOR OBTAINING A WATER-IN-OIL EMULSION BASED ON VEGETABLE OIL AND BUTTER STEARIN

Abstract

The present invention relates to a water-in-oil emulsion comprising no "exotic" concrete fats of vegetable origin and whose fat phase comprises butter or MGLA (CB), MGLA stearin (SB) having a dropping point between 37 and 45 °C, and a vegetable oil (HV); where the mixture (M) of (HV), (SB) and (CB) represents at least 90% by weight of the fat phase with: 1) The proportion (HV) ranging from 20 to 75% (by weight) of the mixture (M), 2) The proportion (SB) ranging from 5 to 65% (by weight) of the mixture (M), 3) The proportion (CB) ranging from 5 to 65% (by weight) of the mixture (M), and 4) The sum (SB) + (CB) ranging from 25 to 80% (by weight) of the mixture (M).

Description

Title of the invention: METHOD FOR OBTAINING A WATER-IN-OIL EMULSION BASED ON VEGETABLE OIL AND BUTTER STEARIN Scope of the invention

[0001] The present invention relates to the field of edible water-in-oil emulsions based on vegetable oils. Technological background of the invention

[0002] The French population, along with New Zealanders, remains one of the world's largest consumers of butter, with 8.2 kg per capita per year. Various types of butter are available on the French market, produced by churning or continuous churning, salted or unsalted, primarily of bovine origin, but also goat's or sheep's milk butters with Protected Designations of Origin (PDOs). Current trends favor a wide range of textures made possible by reduced-fat butter formulations with varying proportions of water, playing on the distinction between winter and summer butters, whose fatty acid compositions differ. It should be noted that only mechanical processes are permitted for transforming cream into butter.

[0003] In the face of the butter market, a large number of products exist to meet societal demand, particularly in France where gastronomy and cooking represent traditional values. Margarines represent the competitive sector, with consumption stabilizing at around 2.7 kg / capita / year. Created in 1869 in France following a competition organized by Napoleon III to replace butter, Hyppolyte MEGE-MOURIES invented an emulsified formulation of beef fat and milk, which he marketed under the name "Margarine." Margarines are water-in-oil emulsions to which additives may be added, and whose lipid phase must be between 10 and 90%.Numerous margarines exist on the market to compete with butter, each associated with a wide variety of tastes, textures, and vegetable oils used, particularly depending on the health claims made and / or recommended by nutritionists. Today, the selection of vegetable oils used (sunflower, high oleic sunflower, rapeseed, olive, flaxseed, and algal oils) allows for a specific ratio of omega-6 fatty acids. A balanced omega-3, as recommended by PANSES. However, it is essential to combine this selection of vegetable oils with one or a mixture of solid fats (in solid form at 15°C) of animal origin (e.g., butter). or of vegetable origin (palm, palm kernel, shea, copra). These concrete fats are essential to structure the margarine and provide the desired techno-functional properties.

[0004] Now, taking ecological issues into account leads to favouring ingredients which, beyond their nutritional value alone, benefit from the most responsible production possible (e.g., without deforestation) and also, whose distance from the place of their use is as reasonable as possible.

[0005] In this context, it is desirable to obtain a water-in-oil emulsion that does not incorporate "exotic" vegetable fats, specifically vegetable fats obtained from crops grown on the European continent. This approach promotes more responsible use of the resource, ensuring regional self-sufficiency in accordance with the "Farm to Fork" strategy.

[0006] To achieve this, it is desirable to obtain a water-in-oil emulsion with a reasonable butter content, but also incorporating vegetable oils with lipid content of interest (unsaturated fats, particularly Omega 3), with the aim of obtaining emulsions with a composition particularly suited to the needs of individuals, all while exhibiting the best possible organoleptic properties. Summary of the invention

[0007] The inventors have demonstrated that a particular butter stearin, which has a dropping point of approximately 40-41 °C, possesses very specific properties. Because of these properties, this stearin can be used as a replacement for exotic solid fats, and in a proportion half that of the fats it replaces, to obtain spreadable fats that have similar textural and organoleptic properties and are perfectly suited to the market.

[0008] Consequently, a first object of the invention relates to a process for producing a water-in-oil emulsion comprising the steps of:

[0009] (i) Preparation of a fatty phase;

[0010] (ii) Preparation of an aqueous phase;

[0011] (iii) Incorporation of the aqueous phase obtained in step (ii) into the oily phase obtained in step (i) under agitation to create an emulsion; and

[0012] (iv) Crystallization of the emulsion obtained in step (iii);

[0013] Characterized in that the fatty phase comprises:

[0014] - no concrete fat of "exotic" vegetable origin;

[0015] - a vegetable oil (VO);

[0016] - of anhydrous milk fat stearin (MFF) (SB) exhibiting a dropping point between 37 and 45 °C; preferably between 38 and 43 °C and, particularly preferably, between 39 and 42 °C; and

[0017] - butter or MGLA (CB), preferably MGLA,

[0018] Where the mixture (M) of (HV), (SB) and (CB) (namely (M) = (HV) + (SB) + (CB) = 100%) represents at least 90% by weight of the oil phase, preferably at least 95% of the oil phase, with:

[0019] 1) The proportion (HV) ranging from 20 to 75% (by weight) of the mixture (M), preferably from 30 to 65%;

[0020] 2) The proportion (SB) ranging from 5 to 65% (by weight) of the mixture (M), preferably of 10 to 40%;

[0021] 3) The proportion (CB) ranging from 5 to 65% (by weight) of the mixture (M), preferably from 25 to 60%; and

[0022] 4) The sum (SB) + (CB) ranging from 25 to 80% (by weight) of the mixture (M), of preference of 35 to 70%.

[0023] The set of emulsions obtained, whose fatty phases are as defined above, then simultaneously exhibit physical and organoleptic properties making them particularly suitable for use as a spreadable fat.

[0024] In addition, the inventors have shown that it was possible to produce such an emulsion, with the same textural and organoleptic properties, but without adding an emulsifier.

[0025] Advantageously, the fatty phase does not include any emulsifier within the meaning of European Regulation No. 1333 / 2008 on additives.

[0026] The present invention also relates to a water-in-oil emulsion that can be obtained by such a process.

[0027] Finally, the invention relates to the use of an MGLA stearin having a dropping point between 37 and 45°C for the manufacture of a water-in-oil emulsion not comprising any "exotic" concrete fat of vegetable origin. Description of the figures

[0028] Fig. 1 represents the endothermal profiles of MGLA and MGLA stearins obtained at different fractionation temperatures.

[0029] Fig. 2 is a geometric (2D) representation of the mixtures produced.

[0030] The [Fig.3] corresponds to the beginning of the positioning of the curves of the same value (isoresponse curve and in a third dimension) of hardness (for chosen hardness values) so as to represent the hardness values ​​of the mixtures in 2D.

[0031] The [Fig.4] is the geometric representation (2D) of the mixtures made incorporating the hardness isoreponse curves (0.9 to 10.90 N). Detailed description of the invention

[0032] The water-in-oil emulsions obtained by the process of the invention are edible.

[0033] Typically, the water-in-oil and oil-in-water emulsions obtained have a fat content of between 10 and 90% (by weight relative to the total weight of the emulsion), preferably between 30 and 70%, particularly between 40 and 60%, and especially preferably between 40 and 55%.

[0034] Preferably, the process of the invention makes it possible to obtain water-in-oil emulsions of the type of spreadable fats and, in particular, margarines.

[0035] The term "spreadable fat" refers to a mixture of water and dairy, animal, and / or vegetable fats, preferably dairy and / or vegetable fats. Examples of such spreadable fats include butter and margarine. The spreadable fats according to the invention can be consumed raw or cooked due to their use in cooking and / or baking.

[0036] Spreadable fats as defined by Regulation (EC) No 2991 / 94) are products whose fat content is a minimum of 10% and a maximum of 90% of their total weight and which retain a solid consistency at 15°C.

[0037] The water-in-oil emulsions obtained have a solid consistency at 15 °C.

[0038] The water-in-oil emulsions obtained have a hardness at 4 °C of between 2 and 18 N, preferably a hardness between 4 and 14 N and, particularly preferably a hardness between 5 and 10 N.

[0039] Such a hardness value at 4 °C is easily determined by a person skilled in the art.

[0040] By way of example, such a hardness is determined using a cylindrical probe 5 mm in diameter, which is positioned more than 10 mm from the side walls of the sample container (to limit edge effects), with the probe penetrating to a length between 30 and 40% of the sample without exceeding a depth of 2 centimeters. Such a hardness can be determined, in particular, as in the examples, with an AGS-X universal measuring machine (SHIMADZU), with the additional parameter setting the probe penetration speed to 1 mm / s and limiting the probe stroke within the sample to 40% of its height. It should also be noted that, in the examples, the sample is aliquoted into a bottle of 60 mL with a height of 70 mm and a diameter of 35 mm; with a sample height of approximately 50 mm.

[0041] In relation to the water-in-oil emulsions according to the invention and for a given hardness (Y), their composition can be determined simply by the following formula:

[0042] Hardness (Ÿ) = -33.365 (HV) - $4.443 (CB) - 164 / 198 (SB) + 321.254 (HV * CB) 4 522.337 (HV * SB) 4 1373.089 (CB « SB) - 3465.38 (HV * CB « SB)

[0043] In which:

[0044] - the hardness (Y) is expressed in Newtons and (HV), (CB) and (SB) are expressed in percentage of their mixture (M) (consisting of the three and with 100% equal to 1);

[0045] - (HV*CB) corresponds to the interaction between vegetable oil and butter or MGLA, and is equal to (HV) x (CB);

[0046] - (HV*SB) corresponds to the interaction between vegetable oil and MGLA stearin, and is equal to (HV) x (SB);

[0047] - (CB*SB) corresponds to the interaction between butter or MGLA and stearin of MGLA, and is equal to (CB) x (SB);

[0048] - (HV*CB*SB) corresponds to the interaction between vegetable oil, butter or the MGLA, and MGLA stearin, and is equal to (HV) x (CB) x (SB).

[0049] In connection with the fat phase and with regard to "exotic" concrete fats of vegetable origin, we mean concrete fats of vegetable origin obtained from crops not grown on the European continent.

[0050] As an example of such "exotic" concrete fats of vegetable origin, one can cite those obtained from coconut (copra), oil palm fruit (palm kernel oil or palm oil), cocoa bean (cocoa butter), sal or sala fruit, nuts of trees of the genus Shorea of ​​the family Dipterocarpaceae (illipe butter), Garcinia indica fruit (kokum butter), or shea fruit (shea butter) and mixtures thereof.

[0051] Anhydrous milk fat (MGLA) is also known as concentrated (solid) butter. It contains at least 99.8% milk fat and has the advantage of being easier to preserve than butter due to its very low water content.

[0052] Stearin of a fat is defined as the solid fraction of that fat, as opposed to the liquid fraction of the same fat, such as olein, which is obtained through fractionation. Typically, this fractionation process takes place at a temperature ranging from 20 to 32 °C, preferably from 25 to 30 °C, and typically around 30 °C. Optionally, this fractionation process may include more than one fractionation step in order to enrich the stearin with saturated fatty acids (SFAs).

[0053] The "dropping point" of a solid fat is defined as the temperature at which the first drop appears. Such a dropping point can be easily determined by a person skilled in the art, in particular by referring to the international standard ISO 6299, which specifies a method for determining the dropping point of a specific fat over a wide temperature range.

[0054] Typically, such an MGLA stearin has a percentage of Saturated Fatty Acids (SFAs) greater than or equal to 65% by weight (relative to its total weight), preferably at least 70% by weight.

[0055] As an example of such a commercially available stearin, MGLA41 (CORMAN) can be cited.

[0056] “Vegetable oil” means a liquid fat at 15 °C. Such a vegetable oil is chosen from the group consisting of sunflower oil, rapeseed oil, maize oil, linseed oil, olive oil, hemp oil (the content of which is delta-9-tetrahydrocannabinol (A9-THC) at the threshold defined by Commission Regulation (EU) 2022 / 1393 of 11 August 2022 amending Regulation (EC) No 1881 / 2006), their fractions, and / or mixtures thereof, preferably from the group consisting of sunflower oil, rapeseed oil and linseed oil and / or mixtures thereof.

[0057] Preferred vegetable oils include essential polyunsaturated fatty acids (PUFAs) such as linoleic acid (LA) from the Omega-6 series, and alpha linolenic acid (ALA) from the Omega-3 series, precursor of eicosapentaenoic acid (EPA) and docosahexaenoic acid (DHA).

[0058] According to a preferred embodiment, the vegetable oil is rapeseed oil.

[0059] Now, it may be a mixture and the vegetable oil then comprises rapeseed oil in a proportion ranging from 20 to 100% by weight (relative to the total weight of the vegetable oil), preferably from 50 to 100% by weight and, particularly preferably, from 70 to 100% by weight.

[0060] In the case of such a mixture and preferably, the vegetable oil may include, in addition to rapeseed oil, sunflower oil and / or linseed oil.

[0061] According to another preferred embodiment, the vegetable oil is sunflower oil.

[0062] Now, it may be a mixture in which the vegetable oil then comprises sunflower oil in a proportion ranging from 20 to 100% by weight (relative to the total weight of the vegetable oil), preferably from 50 to 100% by weight and, particularly preferably, from 70 to 100% by weight.

[0063] In the case of such a mixture and preferably, the vegetable oil may include, in addition to sunflower oil, rapeseed oil and / or linseed oil.

[0064] The oily phase may also contain other hydrophobic compounds such as sources of long-chain Omega-3 fatty acids (e.g., fish oils or microalgae), flavorings, emulsifiers, colorings or vitamins in a proportion not exceeding 10% by weight (relative to the total weight of the fat phase), preferably not exceeding 5%.

[0065] If the oil phase can include one or more emulsifiers to promote the dispersion of the aqueous phase in the oil phase in step (iii) of the process according to the invention, the inventors have shown that the properties of the oil phase defined above are such that the emulsion obtained exhibits very good dispersion, very good organoleptic properties and very good stability without requiring the incorporation of additional emulsifier.

[0066] Also, and according to a preferred embodiment, the fatty phase does not include any emulsifier within the meaning of European Regulation No. 1333 / 2008 on additives.

[0067] Accordingly, the oil phase does not include any emulsifier selected from the group consisting of sodium carboxymethylcellulose (E 466, cellulose gum), cross-linked sodium carboxymethylcellulose (E 468, cross-linked cellulose gum), enzymatically hydrolyzed carboxymethylcellulose (E 469, enzymatically hydrolyzed cellulose gum), sodium, potassium and calcium salts of fatty acids (E 470a), magnesium salts of fatty acids (E 470b), mono- and diglycerides of fatty acids (E 471) and their esters with acetic acid esters of mono- and diglycerides of fatty acids (E 472a), lactic acid esters of mono- and diglycerides of fatty acids (E 472b), citric acid esters of mono- and diglycerides of fatty acids (E 472c), tartaric acid esters of mono- and diglycerides of fatty acids (E 472d),monoacetyl tartaric acid and diacetyl tartaric acid esters of mono- and diglycerides of fatty acids (E 472e), mixed acetic and tartaric acid esters of mono- and diglycerides of fatty acids (E 472f), sucrose esters of fatty acids (E 473), sucroglycerides (E474), polyglycerol esters of fatty acids (E475), polyglycerol polyricinoleate (E 476), propane-1,2-diol esters of fatty acids (E477), heated oxidized soybean oil that has reacted with mono- and diglycerides of fatty acids (E 479b), sodium stearoyl-2-lactylate (E 481), calcium stearoyl-2-lactylate (E 482), stearyl tartrate (E 483), sorbitan monostearate (E 491), sorbitan sadearate (E 492), sorbitan monolaurate (E 493), sorbitan monooleate (E 494) and sorbitan monopalmitate (E 495). ,

[0068] Now, according to a particular embodiment, the fat phase may optionally include lecithins (E322), which act as an anti-splash agent in the margarine. Preferably, the fat phase also does not include any lecithin (E322).

[0069] Step (i) of preparing the oil phase is carried out by techniques well known to those skilled in the art and is typically done under agitation.

[0070] Agitation is preferably carried out by a paddle mixer or by any other system which can meet the requirements of the mixing.

[0071] The preparation temperature is generally between 50 and 70 °C, preferably between 55 and 65 °C.

[0072] As for the aqueous phase this time, it is mainly made up of pure water.

[0073] Now, the aqueous phase can also contain other hydrophilic compounds such as flavorings, colorings, texturizers (e.g., stabilizers, thickeners or gelling agents), preservatives, antioxidants, vitamins, acidity and pH regulators, proteins, milk products (e.g., buttermilk, whey, milk powder), sugars or mineral salts (sodium, calcium, magnesium, ...).

[0074] Step (ii) of preparing the aqueous phase is again carried out using techniques well known to those skilled in the art (e.g., under agitation). Typically, this step is carried out with a paddle mixer or any other system that meets the mixing requirements (deflocculator, propeller, etc.).

[0075] The preparation temperature is generally between 45 and 65 °C, preferably between 50 and 60 °C.

[0076] Step (ii) can be carried out in parallel with step (i), after it or before it.

[0077] Step (iii) of incorporating the aqueous phase into the oily phase is carried out under strong agitation to achieve an emulsion, for example using a paddle shaker or by continuous injection.

[0078] Step (iv) of crystallizing the emulsion corresponds to cooling the emulsion so as to allow its solidification.

[0079] This step is carried out using techniques well known to those skilled in the art and may include pre-cooling the emulsion (so as to obtain a product at a temperature below 50 °C, preferably below 40 °C). Furthermore, this step may include pressurizing the emulsion to facilitate its continuous crystallization (on the order of 1 to 6 MPa). Generally, the emulsion undergoes successive passes through scraped-surface heat exchangers. The passes through the heat exchangers are interspersed with mixing cycles.

[0080] Finally, the outlet temperature of the emulsion at the end of step (iv) is between 5 and 20 °C, preferably between 10 and 15 °C.

[0081] A second object of the invention relates to water-in-oil emulsions that can be obtained by the process described above.

[0082] Advantageously, the water-in-oil emulsion does not include any emulsifier within the meaning of European Regulation No. 1333 / 2008 on additives.

[0083] Thus, such a water-in-oil or oil-in-water emulsion does not comprise any emulsifier selected from the group consisting of sodium carboxymethylcellulose (E 466, cellulose gum), cross-linked sodium carboxymethylcellulose (E 468, cross-linked cellulose gum), enzymatically hydrolyzed carboxymethylcellulose (E 469, enzymatically hydrolyzed cellulose gum), sodium, potassium, and calcium salts of fatty acids (E 470a), magnesium salts of fatty acids (E 470b), mono- and diglycerides of fatty acids (E 471) and their esters with acetic acid esters of mono- and diglycerides of fatty acids (E 472a), lactic acid esters of mono- and diglycerides of fatty acids (E 472b), citric acid esters of mono- and diglycerides fatty acids (E 472c), tartaric acid esters of mono- and diglycerides of fatty acids (E 472d),monoacetyl tartaric acid and diacetyl tartaric acid esters of mono- and diglycerides of fatty acids (E 472e), mixed acetic and tartaric acid esters of mono- and diglycerides of fatty acids (E 472f), sucrose esters of fatty acids (E 473), sucroglycerides (E474), polyglycerol esters of fatty acids (E475), polyglycerol polyricinoleate (E 476), propane-1,2-diol esters of fatty acids (E477), heated oxidized soybean oil that has reacted with mono- and diglycerides of fatty acids (E 479b), sodium stearoyl-2-lactylate (E 481), calcium stearoyl-2-lactylate (E 482), stearyl tartrate (E 483), sorbitan monostearate (E 491), sorbitan sadearate (E 492), sorbitan monolaurate (E 493), sorbitan monooleate (E 494) and sorbitan monopalmitate (E 495). ,

[0084] Advantageously still, the water-in-oil emulsion does not include any lecithin (E322).

[0085] A third object of the invention relates to the use of an MGLA stearin having a dropping point between 37 and 45 °C for the manufacture of a water-in-oil emulsion not comprising any "exotic" concrete fat of vegetable origin.

[0086] Preferably, MGLA stearin has a dropping point between 38 and 43 °C and, particularly preferably, between 39 and 42 °C.

[0087] The following examples are provided for illustrative purposes only and shall not limit the scope of the present invention. Examples

[0088] L _ Obtaining and characterizing an MGLA stearin

[0089] Laboratory-scale mechanical fractionation of MGLA

[0090] As part of this research, the inventors carried out multiple mechanical fractionations of MGLA in order to characterize new raw materials of distinct compositions with a distinct dropping point.

[0091] These mechanical fractionations were carried out at different temperatures (21 °C, 26 °C, 30 °C) so as to separate the olein fraction (liquid) from the stearin fraction (solid) at each of these temperatures.

[0092] To determine the characteristics of each of the stearins obtained, their hardness was measured at 4 °C using the AGS-X universal measuring machine (SHIMADZU), equipped with a 5 mm diameter cylindrical probe. The probe penetrated 40% of the sample height at a speed of 1 mm / s. All samples were aliquoted into 60 mL QUALIOACTT transparent bottles, 70 mm high and 35 mm in diameter, before being placed at 4 °C. The samples were approximately 50 mm high in the bottle.

[0093] The details of the hardness measurements for the different MGLA stearins are listed in Table I below.

[0094] The thermal behavior of the different stearins was further analyzed by Differential Scanning Calorimetry (DSC) using the TA Discovery DSC 2500 (TA INSTRUMENTS). To do this, the instrument was calibrated with respect to enthalpy using indium, the melting point of which is 156.60 °C. Samples (approximately 10 mg) were sealed in TZERO aluminum airtight containers, and an empty container was used as a reference. The system was purged with nitrogen. The analysis was performed starting at -80 °C with a heating step to 80 °C at a rate of 5 °C / min. The results were analyzed using TRIOS V5.0 software (TA INSTRUMENTS).

[0095] The endothermic profiles obtained are presented in [Fig.1].

[0096] From these results, it was also possible to determine the dropping point of the different stearins. For this, the dropping point values ​​are obtained by integrating the endothermic signals in order to obtain the value which represents 95% of the melted fraction for each concrete fat as described in VINCENT et al. (Energy & Fuels, vol.31 (10), p:11489-11494, 2017).

[0097] The details of the dropping points determined for the different MGLA stearins are listed in Table I below (and also the hardness measurements as previously stated). For verification purposes, the hardness values ​​of MGLA, copra, and shea stearin are indicated.

[0098] [Tables 1] Concrete fat content Dropping point (°C) Hardness at 4°C (N) MGLA 32.44 53.37 MGLA stearin with fractionation at 21 °C 21.58 96.56 MGLA stearin with fractionation at 26 °C 36.40 130.06 MGLA stearin with fractionation at 30 °C 40.44 152.09 Copra 23.94 >200 Shea stearin 32.51 >200

[0099] The results show that a hardness of over 100 N is obtained with stearin having a dropping point of 36 °C, and even a hardness of nearly 150 N for stearin having a dropping point of about 40 °C. However, these hardness values ​​remain lower than those of copra or shea stearin.

[0100] Now, the results also show that while MGLA and MGLA stearins with dropping points at approximately 21 and 36 °C exhibit very similar enthalpy change profiles, the profile of MGLA stearin with a dropping point at approximately 40 °C is very different. For the latter, the results show a significantly more pronounced enthalpy change around 40 °C, which temperature approaches that of oral administration.

[0101] Margarine formulations from MGLA stearin obtained by fractionation

[0102] In light of the properties of stearin having a dropping point around 40 °C (in particular compared to those having dropping points of 31 and 36 °C), and in order to better characterize it, the inventors carried out various tests of formulation of water-in-oil emulsions incorporating the latter.

[0103] The process for producing the margarines was as follows:

[0104] Fatty phase;

[0105] 1- The various oils and concrete fats are heated to 55 °C in a thermostatically controlled tank under agitation.

[0106] 2- A gradual increase to a temperature of 80 °C is carried out (at least 5 minutes) before initiating a pasteurization step at 90°C for 20 seconds.

[0107] 3- A cooling step allows the temperature to return to 55 °C.

[0108] Aqueous phase;

[0109] Simultaneously, the aqueous phase with the addition of the various additives and constituents is heated to a temperature of 55 °C for 20 to 30 minutes under agitation to allow complete hydration of the various added constituents, some of which were in powder form.

[0110] Emulsification;

[0111] The aqueous and oily phases (with the aqueous phase representing 48% of the total weight of the emulsion and the oily phase representing 52% of the total weight of the emulsion) are mixed at 55 °C to obtain an emulsion (1500 rpm, 6 minutes).

[0112] Crystallization;

[0113] The emulsion is cooled gradually under agitation (mixing) until the temperature reaches 12-14 °C.

[0114] The product obtained is then placed in trays and then in a cold room at 4-6 °C for the crystallization phase for 24 to 48 hours.

[0115] The composition of the fatty phases (relative to the total weight of the emulsion) for some of the tested emulsions is detailed in Table 2 below; which emulsions incorporate, as a control, an emulsion incorporating copra and shea stearin.

[0116] [Tables2] Fat content Control margarine (g / 100g of product) Tested margarine (g / 100g of product) Rapeseed oil 24.88 24.88 Coconut oil 10.15 - Butter 14.80 14.80 Shea stearin 3.20 - MGLA stearin - 13.35

[0117] The fat phase also included an emulsifier E471 composed of mono- and diglycerides for about 1% by weight (relative to the weight of the fat phase), as well as [3-carotene as a color.

[0118] Preparation of the water-in-oil emulsion

[0119] The aqueous phase, meanwhile, was composed mainly of water with also some food salt, skimmed milk powder, potassium sorbate and lactic acid.

[0120] The preparation of the aqueous phase takes place in a tank equipped with an agitator.

[0121] The oil phase, meanwhile, is carried out in a tank adapted for the phases viscous.

[0122] The aqueous phase is moderately incorporated into the oily phase, under agitation, so as to produce the emulsion.

[0123] The emulsion thus formed is pasteurized to eliminate germs that could alter the microbiological stability of the finished product. The heat treatment is carried out in a scraped-surface heat exchanger.

[0124] Crystallization of the water-in-oil emulsion

[0125] Crystallization and mixing take place successively. The product passes through scraped-surface cooling cylinders to initiate crystallization. Temperature control is automated.

[0126] Cooling, interspersed with mixing steps, is carried out by cylinders whose fingers intertwine to promote homogenization of the product and initiation of crystallization.

[0127] Crystallization continues for several days at 4 °C.

[0128] Hardness of the emulsions obtained

[0129] In order to specify the characteristics of each of the emulsions obtained, the hardness of each of them was determined via the AGS-X universal measuring machine (SHIMADZU) as described previously.

[0130] It emerged that, while the control margarine exhibited an expected hardness of around 6 N at 4 °C, the margarine incorporating stearin with a dropping point of approximately 40 °C showed a significantly higher hardness at 4 °C, on the order of 8.5 N, even though this stearin alone exhibited a lower hardness than the components it replaced (see Table 1). Ultimately, it was possible to obtain a margarine with a hardness similar to that of the control margarine, but by halving the proportion of stearin with a dropping point of approximately 40 °C (compared to the proportions of exotic solid fats used in the control margarine).

[0131] Organoleptic qualities of the emulsion obtained

[0132] Organoleptically, the MGLA stearin-based margarine with a dropping point approaching 40°C exhibited an interesting mouthfeel, similar to butter. Likewise, the buttery aroma was more pronounced and perceptible in this margarine compared to the control.

[0133] Interest of MGLA stearin with a dropping point of around 40 _ °C.

[0134] Ultimately and unexpectedly, the results showed that the physical and organoleptic properties of this MGLA stearin enabled it to effectively replace so-called "exotic" concrete fats (such as coconut and shea stearin for the formulation of spreadable fats). It should be noted that the properties of this stearin allowed it, beyond simply replacing these "exotic" concrete fats, to be used in smaller quantities to obtain similar physical and organoleptic properties (hardness).

[0135] II. _ Characterization of mixtures using this stearin

[0136] To carry out this characterization, a mixture design comprising three components (rapeseed oil, MGLA and MGLA41 (MGLA stearin with a dropping point of 41 °C marketed by CORMAN) was created using NEMRODW software, based on laboratory benchtop fractionation tests of MGLA. In detail, a Doehlert matrix was constructed around a mixture with known proportions of its three components, subject to constraints. The limits of the experimental domain were those detailed in Table 3, which gives the proportions of the three major components (MGLA, vegetable oil, and MGLA stearin) within the oil phase. A geometric representation of the experimental domain of the mixtures was created as illustrated in [Fig. 2].

[0137] [Tables3] Fat content. Range of tested proportions (as a % of the fat phase): Rapeseed oil 39 to 74 mg / L 16 to 50 mg / L 41 10 to 44

[0138] The experimental matrix led to the formulation of a multitude of mixtures in order to precisely determine the influence of each of these 3 constituents and the interactions between them, particularly on firmness. To this end, the hardness at 4°C for each of these formulations was determined as before with the AGS-X universal measuring machine (SHIMADZU).

[0139] The firmness results at 4 °C were then integrated into the geometric representation of the mixtures in a complementary dimension, as illustrated in [Fig. 3]. Finally, the processing of all the results led to a detailed geometric representation in [Fig. 4] illustrating the hardness of the different mixtures (with 2D isoreponse curves obtained by the response surface method).

[0140] In the end, the results made it possible to determine the different mixtures of these 3 major constituents, without any concrete fat of exotic origin but only a particular MGLA stearin, making it possible to obtain (with a significance of 0.01%) a margarine exhibiting, in addition to the desired organoleptic properties, a hardness (Y) expressed in newtons (N), desired at 4°C (depending on the desired texture) by solving the equation of the centered cubic model corresponding to the following formula:

[0141] Hardness (Y) = — 33.365 (HV) - $4.443 (CB) - 164.198 (SB) 4,321.284 (HV * CB) 4,522.337 (HV * SB) 4,1373.089 (CB » SB) - 3465.38 (HV * CB * SB)

[0142] In which:

[0143] [Tables4] Component Value (HV): Proportion of vegetable oil relative to the mixture (M) of vegetable oil, MGLA, and MGLA stearin, expressed as a percentage, with (M) = 1 (corresponds to 100%). (CB): Proportion of MGLA relative to the mixture (M) of vegetable oil, MGLA, and MGLA stearin, expressed as a percentage, with (M) = 1 (corresponds to 100%). (SB): Proportion of MGLA stearin relative to the mixture (M) of vegetable oil, MGLA, and MGLA stearin, expressed as a percentage, with (M) = 1 (corresponds to 100%). (HV*CB): Interaction between vegetable oil and MGLA. (HV) x (CB) (HV*SB): Interaction between vegetable oil and MGLA stearin. (HV) x (SB) (CB*SB): interaction between MGLA and MGLA stearin (CB) x (SB) (HV*CB*SB): interaction between vegetable oil, MGLA and MGLA stearin (HV) x (CB) x (SB)

[0144] The formulation of different emulsions has confirmed that this formula makes it possible to predict the firmness obtained, and therefore to obtain emulsions which, in addition to the organoleptic qualities, have the hardness and therefore the desired texture.

[0145] In addition to obtaining emulsions with interesting organoleptic qualities, the inventors were able to show that this stearin can be used in practically half the quantity of these concrete materials of "exotic" origin to obtain the same firmness at 4 °C.

[0146] 11L _ Characterization of mixtures

[0147] As part of the various experiments and on an exploratory basis, the inventors were led to vary the concentration of emulsifiers (E471) to know its possible impact on the hardness of the emulsions.

[0148] It is in this context and unexpectedly that the inventors observed that this integration of emulsifier showed no significant effect on the hardness of the margarines obtained, even though it normally has significant effects on it.

[0149] In view of the initial results, the inventors more broadly tested different mixtures of the major constituents with and without emulsifiers.

[0150] The results showed that, in similar proportions of the 3 major constituents, the hardness was similar, as were the stability and organoleptic properties.

[0151] Finally, the inventors were able to show that the use of this stearin to obtain a spreadable water-in-oil emulsion makes it possible to do without emulsifiers.

Claims

Demands

1. A process for producing a water-in-oil emulsion comprising the steps of: (i) Preparing a fat phase; (ii) Preparing an aqueous phase; (iii) Incorporating the aqueous phase obtained in step (ii) into the fat phase obtained in step (i) under agitation to create an emulsion; and (iv) Crystallizing the emulsion obtained in step (iii); Characterized in that the fat phase comprises: - no concrete fat of "exotic" vegetable origin; - a vegetable oil (VO); - stearin of anhydrous milk fat (AMF) (AF) having a dropping point between 37 and 45 °C; preferably between 38 and 43 °C and, particularly preferred, between 39 and 42 °C; and - butter or AMF (AF);Where the mixture (M) of (HV), (SB) and (CB) represents at least 90% by weight of the oil phase with: 1) The proportion (HV) ranging from 20 to 75% (by weight) of the mixture (M), 2) The proportion (SB) ranging from 5 to 65% (by weight) of the mixture (M), 3) The proportion (CB) ranging from 5 to 65% (by weight) of the mixture (M), and 4) The sum (SB) + (CB) ranging from 25 to 80% (by weight) of the mixture (M).;

2. The process according to claim 1, characterized in that the concrete fat of "exotic" vegetable origin is selected from those obtained from coconut (e.g. copra), oil palm fruit (e.g. palm kernel oil or palm oil), cocoa bean (e.g. cocoa butter), sal or sala fruit, nuts of trees of the genus Shorea of ​​the family Dipterocarpaceae (e.g. illipe butter), Garcinia indica fruit (e.g. kokum butter), and shea fruit (e.g. shea butter) and mixtures thereof.

3. The process according to any one of claims 1 or 2, characterized in that the vegetable oil is selected from the group consisting of sunflower oil, rapeseed oil, corn oil, linseed oil, olive oil, hemp oil (including the delta-9-tetrahydrocannabinol (A9-THC) content at the threshold defined by Commission Regulation (EU) 2022 / 1393 of 11 August 2022 amending Regulation (EC) No 1881 / 2006), their fractions, and their mixtures.

4. The process according to any one of claims 1 to 3, characterized in that the vegetable oil comprises rapeseed oil in a proportion of 20 to 100% by weight (relative to the total weight of the vegetable oil), preferably 50 to 100% by weight and, in that it may comprise, in addition to rapeseed oil, sunflower oil and / or linseed oil.

5. The process according to any one of claims 1 to 4, characterized in that it is intended for the production of a water-in-oil emulsion having a hardness at 4 °C of between 2 and 18 N, and in that the composition of the emulsion, as a function of its hardness (Y) expressed in newtons (N), can be determined according to the following formula: Hardness (Y) = - 33.365(HV) - 4.443 (CB) - 164.198 (SB) 4 321.254 (HV* CB) 4 522.337(HV * SB) 4 1373.089 (CB * SB) - 3465.38 (HV * CB * SB) in which: 1) the Hardness is expressed in newtons (N) and (HV), (CB) and (SB) are expressed as a percentage of their mixture (M) (with 100% equals 1); 2) (HV*CB) corresponds to the interaction between vegetable oil and butter or MGLA, and is equal to (HV) x (CB); 3) (HV*SB) corresponds to the interaction between vegetable oil and MGLA stearin, and is equal to (HV) x (SB); 4) (CB*SB) corresponds to the interaction between butter or MGLA and MGLA stearin, and is equal to (CB) x (SB);and 5) (HV*CB*SB) corresponds to the interaction between vegetable oil, butter or MGLA, and MGLA stearin, and is equal to (HV) x (CB) x (SB).;

6. The process according to any one of claims 1 to 5, characterized in that the fat phase does not comprise any emulsifier within the meaning of European Regulation No. 1333 / 2008 on additives.

7. The process according to the preceding claim, characterized in that the oil phase does not comprise any emulsifier selected from the group consisting of sodium carboxymethylcellulose (E 466, cellulose gum), crosslinked sodium carboxymethylcellulose (E 468,

8.

9. cross-linked cellulose gum), enzymatically hydrolyzed carboxymethylcellulose (E 469, enzymatically hydrolyzed cellulose gum), sodium, potassium and calcium salts of fatty acids (E 470a), magnesium salts of fatty acids (E 470b), mono- and diglycerides of fatty acids (E 471) and their esters with acetic acid esters of mono- and diglycerides of fatty acids (E 472a), lactic acid esters of mono- and diglycerides of fatty acids (E 472b), citric acid esters of mono- and diglycerides of fatty acids (E 472c), tartaric acid esters of mono- and diglycerides of fatty acids (E 472d), monoacetyl tartaric acid and diacetyl tartaric acid esters of mono- and diglycerides of fatty acids (E 472e) or mixed acetic and tartaric esters of mono- and diglycerides of fatty acids (E 472f), sucrose esters of fatty acids (E 473), sucroglycerides (E474), polyglycerol esters of fatty acids (E475), polyglycerol polyricinoleate (E 476),propane-1,2-diol esters of fatty acids (E477), heated oxidized soybean oil reacted with mono- and diglycerides of fatty acids (E479b), sodium stearoyl-2-lactylate (E481), calcium stearoyl-2-lactylate (E482), stearyl tartrate (E483), sorbitan monostearate (E491), sorbitan tristearate (E492), sorbitan monolaurate (E493), sorbitan monooleate (E494) and sorbitan monopalmitate (E495). A water-in-oil emulsion that can be obtained by the process according to any one of claims 1 to 7. The use of an MGLA stearin having a dropping point between 37 and 45 °C for the manufacture of a water-in-oil emulsion not comprising any "exotic" concrete fat of vegetable origin as defined in the preceding claim.

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