BR102020026665A2 - LIPID COMPOSITION, MACAUBA OIL-BASED LIPID FORMULATIONS AND USES - Google Patents

Abstract

LIPID COMPOSITION, MACAUBA OIL-BASED LIPID FORMULATIONS AND USES. The present invention relates to lipid composition, lipid formulations based on refined macauba pulp oil and fully hydrogenated macauba almond oil and their uses. The present invention has application in food, and the use of the composition and lipid formulations are applicable in pasta in general, among others and cosmetics.

Description

LIPID COMPOSITION, MACAUBA OIL-BASED LIPID FORMULATIONS AND USES field of invention

[1] The present invention relates to lipid composition, lipid formulations based on refined macauba pulp oil and fully hydrogenated macauba almond oil and their uses.

[2] The present invention has application in food and cosmetics.

Fundamentals of the invention

[3] Lipids are substances of animal, vegetable or microbial origin that have the characteristic of solubility in organic solvents and insolubility in water. Its major compound is triacylglycerol (triesters of fatty acids and glycerol), representing about 97% in a crude oil and >99% in a refined oil. Minority compounds present in lipids are diacylglycerols, monoacylglycerols, free fatty acids, waxes, phospholipids, sphingolipids, glycolipids, terpenes, sterols, tocopherols and carotenoids.

[4] When liquids at room temperature are called oils, and when solids, semi-solids or plastics at room temperature are known as fats.

[5] The tendency to modify the structure of oils and fats has increased due to the need to transform liquid oils into solid, semi-solid or plastic fats, with different compositions and physical characteristics, resulting in different application profiles and, therefore, being important constituents of formulations for the chemical, pharmaceutical and food industries. The hydrogenation process consists of adding hydrogen atoms to the double bond of unsaturated fatty acids. The partial hydrogenation process, in which the double bond is not fully hydrogenated, enables the formation of trans fatty acids, known worldwide to be a causative factor in cardiovascular diseases. The partial hydrogenation process will be prohibited in Brazil from the beginning of 2023 through RDC no332, being allowed to use only the total hydrogenation process. In the total hydrogenation process, the double bond of unsaturated fatty acids is completely broken, resulting in a fat with a high melting point and a high content of trisaturates. In this context, interesterification has established itself as an industrial alternative for obtaining structured lipid bases without trans fatty acids. The structure of lipids can be modified through the reorganization of fatty acids in the triacylglycerol main chain through the process of interesterification.

[6] Through interesterification, lipid bases or products with properties different from the raw materials used in the process are obtained. The properties of interesterified products are evaluated through analytical methods that, together, analyze the chemical composition and the general properties of consistency and crystallization.

[7] Macaúba (Acrocomia aculeata) is a highly productive oil palm belonging to the Arecaceae family, native to South America and with higher concentrations in Brazil in the Southeast and Midwest regions. It is popularly known as: macaúba, macaíba, macaiúva, mocajá, mocujá, mucajá, bacaiúva, bocaiuva, coco-de-catarro, coco-de-thorn, imbocaiá, umbocaiuva, depending on the region of its occurrence. Its productivity yields between 1,500 and 5,000 kilos of oil per hectare per year, being considered the second largest source of oil after palm oil. According to some studies, (2013) the macaúba fruit consists of approximately 20% of peel, 40% of pulp, 33% of endocarp and 7% of almond, having two types of economically important oils, stored in the almond and in the pulp. Almond oil is characterized by the predominance of oleic acid and lauric acid and has a translucent appearance. The pulp oil has an orange color, is characterized by a high concentration of oleic acid and high levels of carotenoids, characteristics that possibly imply good oxidative stability.

[8] Due to the predominance of the Macaúba palm (Acrocomia aculeata), in the Brazilian Cerrado and Pantanal and with its use below its real potential, the importance of studying the lipid fractions of the macaúba fruit for industrial application is highlighted. .

[9] After the development and study of formulations containing refined macaúba pulp oil (MPO) and fully hydrogenated macaúba almond oil (FHMKO) before and after the technological process of chemical interesterification, it was possible to direct the application of the lipid bases obtained in foods. The choice of macaúba as raw material for this work was based on its added value, high productivity, several areas of application, such as the cosmetic, food and pharmaceutical industry and lipid composition.

[10] Lüdtke's (2016) master's dissertation entitled "Study of degumming and clarification of crude oil from rice bran (Oryza sativa) for physical refining" reveals that rice is one of the most consumed cereals in the world, mainly in the form of grain. The processing generates by-products, such as rice bran, from which crude rice oil is obtained. Due to the presence of phospholipids, gums, waxes, this oil has a dark color and higher viscosity when compared to other vegetable oils. Furthermore, it contains 1-2% of γ-oryzanol, a compound absent in other oils, which has been attributed antioxidant and hypocholesterolemic effects. The refining method modifies the composition of the oil, in chemical refining, there are significant losses of components during the process, in physical refining the loss of these components is minimized, but it is necessary that the oil arrives at the deodorization stage with a lower phosphorus content. at 10 mg.kg-1, so that physical refining can be carried out. The objective of the dissertation was to carry out studies on degumming, in order to make it suitable for physical refining, and on clarification, so that it is attractive to the consumer. Clarifying activity tests were carried out using two clarifying earths; degumming with water (0.6 and 5%) and phosphoric (0.2%) and citric (0.5%) acids; and clarification tests using the soils and proportions that showed the best clarifying activity. Degumming with 5% water reduced the phosphorus content to values lower than 10 mg.kg-1. Thus, degumming with 5% of water, followed by clarification using citric acid (50%) in the proportion of 0.5% and addition of 2.0% of the clarifying earth, provided an oil suitable for physical refining and with the physical characteristics -chemicals similar to crude oil and within the requirements specified by legislation. Furthermore, it presents several steps similar to those of the present invention: clarification with clarifying earths, added in different proportions (1.0; 1.5; and 2.0%); degumming with water (0.6 and 5%) and citric acid (0.5%).

[11] The present invention differs from the prior art document in that the source used for refining is crude rice bran oil (Orysa sativa). Meanwhile, the present invention relates to macauba oil. The phosphorus content of rice oil was above 200 mg.kg-1, indicating the need for a degumming step with water, which was not necessary in the refining process described for the refining of macaúba oil. In addition, rice oil has high levels of phosphoglycolipids, making the degumming step difficult. The great difficulty of removing phospholipids in a conventional degumming with water due to the presence of phosphoglycolipids. This difficulty was not encountered in the refining of macaúba oils. Furthermore, the refining process with some modifications is already a process widely used in all vegetable oils.

[12] The doctoral dissertation by Queiroz, Lorena Aires Lombardi (2016) entitled "Analysis of Post-Harvest Procedures for Macaúba Fruit (Acrocomia aculeata) and Pulp Oil Refining" reveals that the consumption of vegetable oils has increased worldwide and currently its market is determined not only by consumption for food purposes and production of drugs and lubricants, but also for the production of biodiesel. Macaúba (Acrocomia aculeata), a palm tree typical of the Brazilian Cerrado, produces a fruit that can be used as a source of vegetable oil. You can make full use of all parts of its fruits. However, the most economically representative product are the oils extracted from the pulp and almond. This work had two objectives: 1) the analysis of collection methodologies and post-harvest procedures and 2) the identification of conditions of the refining process, aiming at obtaining pulp oil compatible with the standard established by ANVISA for vegetable oils. An increase in the oil content of the fruits kept in the bunch was detected to values from 43.43% to 52.94% (dry basis), in the 36 days, and after 19 days the value was 50.71%. The evaluation of the refining process for an oil extracted from Macaúba pulp with an initial acidity value of 4.1 mg KOH/g, included the steps of degumming and neutralization, as well as clarification by two alternative processes, the first conventional by adsorption with commercial land. The most used degumming method consists of adding 1% to 3% of water to the crude oil heated at 60° and 70°C, under constant stirring, for 20 to 30 minutes. The precipitate formed is removed from the oil by centrifugation. Furthermore, the study reveals that the adsorbents used in the clarification of oils are predominantly natural or activated clays (or earths) obtained through acid treatment, hydrated aluminum or magnesium silicates and, to a lesser extent, activated carbon, and a combination of activated carbon and clarifying clay. The deodorization step consists of steam distillation, in which volatile substances are removed in a high vacuum. The refining process proposed in the work used chemical refining in which the oil was subjected to a stage of neutralization with sodium hydroxide solution, generating the formation of soaps in which a high volume of water is used in the washing process.

[13] In relation to the present invention, the physical refining process was used for both the pulp and macauba kernel oil, in which it cannot be compared with the chemical refining process since the neutralization step is not used, in addition to the removal of free fatty acids being carried out in the deodorization/distillation step. The proposed technology does not generate soaps as a by-product and consequently does not use water. The present invention used chemical refining and because it presents the neutralization step, it is considered an ecologically incorrect process and in the near future, it tends to go into disuse. The use of physical refining, a route considered by the area of oils and fats, as a "clean" and ecologically appropriate process.

[14] The study by Angela Alves Nunes, Simone Palma Favaro and Simone Mendonça (2013), entitled "MACAÚBA PULP OIL REFINING PROCESS: IDENTITY AND QUALITY PROPERTIES", declares that the demand for vegetable oils is growing, leveraged , above all, for consumption in the food market. Macaúba (Acrocomia aculeata (Jacq) Lood. ex Mart.) fruits can produce similar amounts of oil to palm oil, which means ten times more oil than soybeans per area. The refining process is usually carried out in sequence (degumming, neutralization, bleaching and deodorization) in order to eliminate, completely or partially, these substances that affect the color, stability, aroma and flavor of the oils.

[15] Differently, the present invention refers to a process for refining crude macauba oil that comprises the steps: degumming, neutralization, bleaching and deodorization. The first step consisted of degumming the oil by adding distilled water in the proportion (1:2) water:oil. The neutralization of free fatty acids was by means of the addition of an aqueous solution of sodium hydroxide equivalent to 6 °Baumé. Bleaching was performed with 10% activated earth treatment (Oil:dri brand, Supreme ProActive model) (m/m). The process for deodorizing the bleached oil was steam stripping under vacuum. In this way, refined macaúba pulp oil is obtained. The objective of this work was to extract, characterize and chemically refine on bench scale and evaluate macaúba pulp oil, considering the quality and identity standards established by other oil sources. Thus, the work used the chemical refining route, in which it presents the neutralization step. In addition, the degumming step was mentioned without the results in the phosphorus content, in addition to the use of 10% of activated earth, which does not match the reality of the market, whose maximum content used is 1%. In comparison, the present invention used the physical refining route, which does not include the neutralization step.

[16] The scientific article by ZEITOUN, M. A. M.; NEFF, W.E.; LIST, G.R.; MOUNTS, T. L. Physical properties of interesterified fat blends. Journal Of The American Oil Chemists' Society, [s.l.], v. 70, no. 5, p. 467-471 (1993) entitled "Physical properties of interesterified fat blends" reports the chemical interesterification of fully hydrogenated soybean oil, with canola, soybean, sunflower, cotton, corn, palm, peanut, safflower and coconut oil, in the proportion of 1:1. Under reaction conditions of 60 min, 95 °C and 0.3% sodium methoxide. The results indicated that palm and cotton oils, with a high content of palmitic acid (C16:0), were related to the solids profile and crystallization behavior typical of traditional margarines. In the work, mixtures of 9 different types of vegetable oils with totally hydrogenated soybean oil were used in the proportion of 1:1 (m/m) submitted to chemical interesterification reaction and the fractions were evaluated before and after the modification process. The following vegetable oil sources were used: palm, coconut, cotton, peanut, soybean, corn, sunflower, safflower and canola. The interesterification process is consolidated in the area of oil and fat technology and is considered one of the main alternatives for modifying vegetable oils and is widely used for various raw materials. Unlike the present invention, the work did not use refined and fully hydrogenated macaúba oils.

[17] In a work published by FÁVARO, (2013) entitled "Refining process of macaúba pulp oil", crude macaúba pulp oil, within the quality standards required for this category, goes through the steps of degumming, neutralization , bleaching and deodorization. Under the conditions used, refined oil is obtained that meets the quality criteria required for vegetable oils by legislation. The document reports the main stages of the specific oil refining process for macaúba oil. However, without presenting the specific conditions to the present creation. The document does not mention the extraction process and refining condition, but mentions the steps used in chemical refining involving degumming, neutralization, bleaching and deodorization. The work utilized a refining route distinct from the present invention. Chemical refining, due to the neutralization stage, is considered an ecologically incorrect process and, in the near future, it tends to fall into disuse. The use of physical refining, a route considered by the area of oils and fats, as a "clean" and ecologically appropriate process.

[18] In the present invention, the chemical interesterification reaction was effective for all formulations developed, as it altered the physical properties, promoted a decrease in the melting point and in the crystallization kinetics. The fatty acid composition of fully hydrogenated macaúba pulp oil and almond oil provided the formation of triacylglycerols with a wide range of carbon numbers (C30 to C54) and directly influenced the thermal behavior of the lipid formulations of the present invention.

[19] Even with the presence of trisaturated triacylglycerols, the lipid formulations showed a reduction in consistency due to a reduction in the melting point, related to the formation of triacylglycerols of intermediate molecular weight and a decrease in triacylglycerols with higher molecular weight with a consequent decrease in ΔΤ (oC ) both crystallization and melting. The lipid formulations showed mixtures of β' and β crystals and uniform and structured crystalline networks.

[20] Aiming at the application of the lipid formulations of the present invention, the lipid bases were characterized as extremely hard, which can make it difficult to apply them alone in foods at refrigeration temperature (15°C). At 25°C, the lipid formulations showed satisfactory results in terms of plasticity and spreadability, being able to be applied in different products. Interesterified lipid bases with higher thermal resistance (35°C) showed adequate spreadability behavior.

[21] Finally, it is concluded that lipid formulations can be directed to the application of lipid-based products introducing the unprecedented fractions of macaúba oil in foods.

Brief description of the invention

[22] The present invention relates to lipid composition, lipid formulations based on refined macauba pulp oil and fully hydrogenated macauba kernel oil and their uses.

• - 15 a 72% de SFC em 20 oC;
• - 8 a 56% de SFC em 25 oC;
• - 4 a 38% de SFC em 30 oC

- Ponto de fusão: 30 e 41 °C;
- Cinética de cristalização:

• - tSFC: 5 a 10 minutos;
• - SFCmáx: 12,75 a 60,41%;
• - t1/2SFCmáx: 15 a 22 minutos;

- Consistência (Yield Value (YV):

• - a 15 °C: 1938,79 a 25546,10 gF/cm2; e
• - a 25 °C: 644,04 a 14976,87 gF/cm2; e
• - a 35 °C: 0 a 1877, 81 gF/cm2.

[23] The lipid composition and lipid formulations are based on refined macauba pulp oil and fully hydrogenated macauba kernel oil and comprise:
- 40% to 100% FHMKO;
- 0% to 60% of MPO;
- 0.36% to 0.94% sodium methoxide;
- Solid fat content:

• - 15 to 72% SFC at 20 oC;
• - 8 to 56% SFC at 25 oC;
• - 4 to 38% SFC at 30°C

- Melting point: 30 and 41 °C;
- Crystallization kinetics:

• - tSFC: 5 to 10 minutes;
• - SFCmax: 12.75 to 60.41%;
• - t1/2SFCmax: 15 to 22 minutes;

- Consistency (Yield Value (YV):

• - at 15°C: 1938.79 to 25546.10 gF/cm 2 ; and
• - at 25°C: 644.04 to 14976.87 gF/cm 2 ; and
• - at 35°C: 0 to 1877, 81 gF/cm 2 .

[24] It is an additional object to use the composition and lipid formulations to be applicable in doughs in general such as cookies, breads and cakes, filled cookies, fillings, light creams, margarines, candies, chocolate toppings, cocoa butter substitutes (CBS ), ice cream toppings, among others.

Brief description of figures

[25] Figure 1 shows the graph with the result of the solid fat content of all formulations developed before (a) the chemical interesterification process.

[26] Figure 2 shows the graph with the result of the solid fat content of all formulations developed after (d) the chemical interesterification process.

[27] Figure 3 shows the graph with the result of the crystallization kinetics of all formulations developed before (a) the chemical interesterification process.

[28] Figure 4 shows the graph with the result of the crystallization kinetics of all formulations developed after (d) the chemical interesterification process.

[29] Figure 5 shows the diffractogram of all formulations developed before (a) the chemical interesterification process at 25oC for 24 hours.

[30] Figure 6 shows the diffractogram of all formulations developed after (d) the chemical interesterification process at 25oC for 24 hours.

[31] Figure 7 shows the consistency graph at 15oC expressed in Yield Value of all formulations developed before (a) and after (d) the chemical interesterification process.

[32] Figure 8 shows the consistency graph at 25oC expressed in Yield Value of all formulations developed before (a) and after (d) the chemical interesterification process.

[33] Figure 9 shows the consistency graph at 35oC expressed in Yield Value of all formulations developed before (a) and after (d) the chemical interesterification process.

[34] Figure 10 shows the consistency graph at 15oC, 25oC and 35oC expressed in Yield Value of the formulation with 100% fully hydrogenated macaúba almond oil before (a) and after (d) the chemical interesterification process .

[35] Figure 11 shows all formulations in simple mixtures, before the reaction, and interesterified, after the lipid modification reaction.

[36] Figure 12 shows the comparison of all formulations before and after the interesterification reaction.

Detailed description of the invention

[37] The present invention relates to lipid composition, lipid formulations based on refined macauba pulp oil and fully hydrogenated macauba kernel oil and their uses.

[38] In the present invention, the macaúba pulp oil is termed as MPO and the fully hydrogenated macaúba kernel oil as FHMKO.

[39] In the present invention the crystallization induction time is termed as tSFC, crystallization half-life time (time required for the sample to reach half the total solids in stabilization) is termed as t1/2SFCmax and the solids content maximum is referred to as SFCmax.

• - 15 a 72% de SFC em 20 oC;
• - 8 a 56% de SFC em 25 oC;
• - 4 a 38% de SFC em 30 oC

- Ponto de fusão: 30 e 41 °C;
- Cinética de cristalização:

• - tSFC: 5 a 10 minutos;
• - SFCmáx: 12,75 a 60,41%;
• - t1/2SFCmáx: 15 a 22 minutos;

- Consistência (Yield Value (YV):

• - a 15 °C: 1938,79 a 25546,10 gF/cm2; e
• - a 25 °C: 644,04 a 14976,87 gF/cm2; e
• - a 35 °C: 0 a 1877, 81 gF/cm2.

[40] The lipid composition based on refined macauba pulp oil and fully hydrogenated macauba kernel oil comprises:
- 40% to 100% FHMKO;
- 0% to 60% of MPO;
- 0.36% to 0.94% sodium methoxide;
- Solid fat content:

• - 15 to 72% SFC at 20 oC;
• - 8 to 56% SFC at 25 oC;
• - 4 to 38% SFC at 30°C

- Melting point: 30 and 41 °C;
- Crystallization kinetics:

• - tSFC: 5 to 10 minutes;
• - SFCmax: 12.75 to 60.41%;
• - t1/2SFCmax: 15 to 22 minutes;

- Consistency (Yield Value (YV):

• - at 15°C: 1938.79 to 25546.10 gF/cm 2 ; and
• - at 25°C: 644.04 to 14976.87 gF/cm 2 ; and
• - at 35°C: 0 to 1877, 81 gF/cm 2 .

[41] Lipid formulations based on refined macaúba pulp oil and fully hydrogenated macaúba kernel oil are named F40, F50, F60, F70, F80, F90 and F100.

• - 15% de SFC em 20 oC;
• - 8% de SFC em 25 oC;
• - 4% de SFC em 30 oC;

- Ponto de fusão: 30 oC;
- Cinética de cristalização:

• - tSFC: 10 minutos;
• - SFCmáx: 12,75%;
• - t1/2SFCmáx: 22 minutos;

- Consistência (Yield Value (YV):

• - a 15 oC: 3191,63 gF/cm2; e
• - a 25 oC: 644, 04 gF/cm2.

[42] The F40 lipid formulation comprises 40% FHMKO, 60% MPO, 0.58 sodium methoxide and the following characteristics:
- Solid fat content:

• - 15% SFC at 20°C;
• - 8% SFC at 25 oC;
• - 4% SFC at 30°C;

- Melting point: 30 oC;
- Crystallization kinetics:

• - tSFC: 10 minutes;
• - SFCmax: 12.75%;
• - t1/2SFCmax: 22 minutes;

- Consistency (Yield Value (YV):

• - at 15°C: 3191.63 gF/cm 2 ; and
• - at 25 oC: 644.04 gF/cm2.

• - 25% de SFC em 20 oC;
• - 12% de SFC em 25 oC;
• - 6% de SFC em 30 oC

- Ponto de fusão: 33 °C;
- Cinética de cristalização:

• - tSFC: 9 minutos;
• - SFCmáx: 19,74%;
• - t1/2SFCmáx: 18 minutos;

- Consistência (Yield Value (YV):

• - a 15 oC: 1938,79 gF/cm2;
• - a 25 oC: 268,57 gF/cm2; e
• - a 35 °C: 35,36 gF/cm2.

[43] The F50 lipid formulation comprises 50% FHMKO, 50% MPO, 0.65 sodium methoxide and the following characteristics:
- Solid fat content:

• - 25% SFC at 20°C;
• - 12% SFC at 25°C;
• - 6% SFC at 30°C

- Melting point: 33 °C;
- Crystallization kinetics:

• - tSFC: 9 minutes;
• - SFCmax: 19.74%;
• - t1/2SFCmax: 18 minutes;

- Consistency (Yield Value (YV):

• - at 15°C: 1938.79 gF/cm 2 ;
• - at 25°C: 268.57 gF/cm 2 ; and
• - at 35°C: 35.36 gF/cm 2 .

• - 33% de SFC em 20 oC;
• - 20% de SFC em 25 oC;
• - 10% de SFC em 30 oC

- Ponto de fusão: 35 °C;
- Cinética de cristalização:

• - tSFC: 7 minutos;
• - SFCmáx: 26,53%;
• - t1/2SFCmáx: 19 minutos;

- Consistência (Yield Value (YV):

• - a 15 oC: 3071,76 gF/cm2;
• - a 25 °C: 1058,21 gF/cm2; e
• - a 35 °C: 82,81 gF/cm2.

[44] The F60 lipid formulation comprises 60% FHMKO, 40% MPO, 0.70 sodium methoxide and the following characteristics:
- Solid fat content:

• - 33% SFC at 20°C;
• - 20% SFC at 25°C;
• - 10% SFC at 30°C

- Melting point: 35 °C;
- Crystallization kinetics:

• - tSFC: 7 minutes;
• - SFCmax: 26.53%;
• - t1/2SFCmax: 19 minutes;

- Consistency (Yield Value (YV):

• - at 15°C: 3071.76 gF/cm 2 ;
• - at 25°C: 1058.21 gF/cm 2 ; and
• - at 35°C: 82.81 gF/cm 2 .

• - 42% de SFC em 20 oC;
• - 28% de SFC em 25 oC;
• - 15% de SFC em 30 oC

- Ponto de fusão: 37,5 °C
- Cinética de cristalização:

• - tSFC: 7 min;
• - SFCmáx: 34,00%;
• - t1/2SFCmáx: 16 min;

- Consistência (Yield Value (YV):

• - a 15 oC: 4108,16 gF/cm2;
• - a 25 °C: 1554,59 gF/cm2; e
• - a 35 °C: 146, 97 gF/cm2.

[45] The F70 lipid formulation comprises 70% FHMKO, 30% MPO, 0.76 sodium methoxide and the following characteristics:
- Solid fat content:

• - 42% SFC at 20°C;
• - 28% SFC at 25°C;
• - 15% SFC at 30°C

- Melting point: 37.5 °C
- Crystallization kinetics:

• - tSFC: 7 min;
• - SFCmax: 34.00%;
• - t1/2SFCmax: 16 min;

- Consistency (Yield Value (YV):

• - at 15°C: 4108.16 gF/cm 2 ;
• - at 25°C: 1554.59 gF/cm 2 ; and
• - at 35°C: 146.97 gF/cm 2 .

• - 53% de SFC em 20 oC;
• - 38% de SFC em 25 oC;
• - 20% de SFC em 30 oC

- Ponto de fusão: 39 °C;
- Cinética de cristalização:

• - tSFC: 7 minutos;
• - SFCmáx: 47,52%;
• - t1/2SFCmáx: 16 minutos;

- Consistência (Yield Value (YV):

• - a 15oC:4900, 09 gF/cm2;
• - a 2 5oC:22 57,2 5 gF/cm2; e
• - a 35oC:263, 17 gF/cm2.

[46] The F80 lipid formulation comprises 80% FHMKO, 20% MPO, 0.82 sodium methoxide and the following characteristics: - Solid fat content:

• - 53% SFC at 20°C;
• - 38% SFC at 25°C;
• - 20% SFC at 30°C

- Melting point: 39 °C;
- Crystallization kinetics:

• - tSFC: 7 minutes;
• - SFCmax: 47.52%;
• - t1/2SFCmax: 16 minutes;

- Consistency (Yield Value (YV):

• - at 15°C: 4900, 09 gF/cm 2 ;
• - at 25°C: 22 57.25 gF/cm 2 ; and
• - at 35°C: 263, 17 gF/cm 2 .

• - 62% de SFC em 20 oC;
• - 46% de SFC em 25 oC;
• - 25% de SFC em 30 oC

- Ponto de fusão: 40 °C;
- Cinética de cristalização:

• - tSFC: 6 minutos;
• - SFCmáx: 49,81%;
• - t1/2SFCmáxx: 15 minutos;

- Consistência (Yield Value (YV):

• - a 15oC:6631,17 gF/cm2;
• - a 2 5oC:37 68,16 gF/cm2; e
• - a 35oC:391,05 gF/cm2.

[47] The F90 lipid formulation comprises 90% FHMKO, 10% MPO, 0.88 sodium methoxide and the following characteristics:
- Solid fat content:

• - 62% SFC at 20°C;
• - 46% SFC at 25°C;
• - 25% SFC at 30°C

- Melting point: 40 °C;
- Crystallization kinetics:

• - tSFC: 6 minutes;
• - SFCmax: 49.81%;
• - t1/2SFCmax: 15 minutes;

- Consistency (Yield Value (YV):

• - at 15°C: 6631.17 gF/cm 2 ;
• - at 25°C: 37 68.16 gF/cm 2 ; and
• - at 35°C: 391.05 gF/cm 2 .

• - 72% de SFC em 20 oC;
• - 56% de SFC em 25 oC;
• - 38% de SFC em 30 oC

- Ponto de fusão: 41 °C
- Cinética de cristalização:

• - tSFC: 5 minutos;
• - SFCmáx: 60,41%;
• - t1/2SFCmáx: 15 minutos;

- Consistência (Yield Value (YV):

• - a 15oC:25546, 10 gF/cm2;
• - a 2 5oC:14976, 87 gF/cm2; e
• - a 35oC:1877, 81 gF/cm2.

[48] The F100 lipid formulation comprises 100% FHMKO, 0.36 sodium methoxide and the following characteristics:
- Solid fat content:

• - 72% SFC at 20 oC;
• - 56% SFC at 25°C;
• - 38% SFC at 30°C

- Melting point: 41 °C
- Crystallization kinetics:

• - tSFC: 5 minutes;
• - SFCmax: 60.41%;
• - t1/2SFCmax: 15 minutes;

- Consistency (Yield Value (YV):

• - at 15°C: 25546, 10 gF/cm 2 ;
• - at 25°C: 14976, 87 gF/cm 2 ; and
• - at 35°C: 1877, 81 gF/cm 2 .

• - óleo da polpa (MPO) e amêndoa de macaúba (FHMKO);
• - Degomagem: adição de 0,1 a 0,6% de ácido cítrico a 50%, com um tempo de permanência de 20 a 30 minutos de contato, seguido de vácuo com pressão variável entre 20 e 30 mmHg com aumento de temperatura para 50°C a 100°C;
• - Clarificação: adição de 0,5 a 1,5% de Tonsil Supreme 1800FF Clariant, preferencialmente 1%, com 25 a 35 minutos de contato, de 85°C a 95°C sob vácuo e posterior filtração em sistemas de filtros com membranas;
• - Destilação/Desodorização: Temperatura de 220°C a 240°C, por 6 a 10 horas, sob vácuo de 7 a 10 mmHg, com injeção de vapor superaquecido;

2) Hidrogenação total:

• - 6 a 10 mbar de pressão;
• - 0,10% a 0,20% de catalisador, preferencialmente níquel comercial;
• - 180°C a 250°C;
• - 4 a 5 horas com separação do níquel através de filtração em membranas;
• - resfriamento até atingir a temperatura entre 70 e 80°C;
• - filtração em filtros de membrana;

3) Interesterificação química:

• - Adição de metóxido de sódio à fase lipídica sob vácuo com elevação a 100°C por 20 minutos;
• - Reação sob alta temperatura, agitação e vácuo: 95°C a 105oC, 450 a 550 rpm;
• - Adição de ácido cítrico: 0,1% v/v de ácido cítrico 5%;
• - lavagem com a utilização de água quente e remoção de sabões com fenolftaleína.
• - Secagem a vácuo com temperatura entre 90°C a 100°C e agitação de 450 a 550 rpm;
• - Teor do catalisador metóxido de sódio: 0,36% a 0,94%; e

4) Obtenção das formulações lipídicas do óleo de macaúba interesterificado.[49] The process of preparing the lipid formulations was carried out as follows:
1) Physical refinement:

• - pulp oil (MPO) and macaúba almond (FHMKO);
• - Degumming: addition of 0.1 to 0.6% of 50% citric acid, with a residence time of 20 to 30 minutes of contact, followed by vacuum with variable pressure between 20 and 30 mmHg with temperature increase to 50 °C to 100 °C;
• - Clarification: addition of 0.5 to 1.5% of Tonsil Supreme 1800FF Clariant, preferably 1%, with 25 to 35 minutes of contact, from 85°C to 95°C under vacuum and subsequent filtration in membrane filter systems ;
• - Distillation/Deodorization: Temperature from 220°C to 240°C, for 6 to 10 hours, under vacuum of 7 to 10 mmHg, with injection of superheated steam;

2) Total hydrogenation:

• - 6 to 10 mbar pressure;
• - 0.10% to 0.20% of catalyst, preferably commercial nickel;
• - 180°C to 250°C;
• - 4 to 5 hours with nickel separation through membrane filtration;
• - cooling until reaching a temperature between 70 and 80°C;
• - filtration in membrane filters;

3) Chemical interesterification:

• - Addition of sodium methoxide to the lipid phase under vacuum with elevation at 100°C for 20 minutes;
• - Reaction under high temperature, agitation and vacuum: 95°C to 105°C, 450 to 550 rpm;
• - Addition of citric acid: 0.1% v/v of 5% citric acid;
• - washing using hot water and removing soaps with phenolphthalein.
• - Vacuum drying at a temperature between 90°C to 100°C and agitation from 450 to 550 rpm;
• - Content of sodium methoxide catalyst: 0.36% to 0.94%; and

4) Obtaining the lipid formulations of interesterified macaúba oil.

[50] After the interesterification process, the formulations showed a melting profile more suitable for applications such as fillings for cookies, margarine and never being used in isolation.

[51] In addition, interesterified lipid formulations containing refined pulp oil and fully hydrogenated almond oil showed different melting profiles from existing bases on the market, which use different sources such as soybean, cotton, palm and palm kernel.

[52] Also, all formulations have a trans fatty acid content of less than 2% since the partial hydrogenation process was not used.

[53] It is important to note that according to RDC 332/2019 published by the National Health Surveillance Agency (ANVISA), the use of partially hydrogenated fats will be banned by 2023 due to the impact on consumer health. In this way, the formulations are in accordance with current legislation not only in Brazil, but also in the whole world.

Step 1: Physical refining

[54] The purpose of refining is to remove unwanted products present in the crude oil, reduce the level of pigments, preserve tocopherols and tocotrienols, reduce the loss of triacylglycerols and protect the oil from degradation.

[55] The parameters of choice between physical and chemical refining are related to the contents of free fatty acids and phospholipids in the crude oil.

[56] In this context, physical refining was selected because it also presents a very positive environmental issue, since there is no use of water during the process, in addition to the disposal of soaps, phospholipids, free fatty acids and losses of neutral oil.

Step 2: Total hydrogenation

[57] The objective of the total hydrogenation process is the transformation of liquid oils into solid, semi-solid or plastic fats, aiming at the structuring of lipid bases with high melting points.

[58] The insertion of hydrogen in the double bond of unsaturated fatty acids promotes their total saturation, without the presence of trans fatty acids.

Step 3: Chemical interesterification

[59] The purpose of chemical interesterification is to obtain new lipid bases, with different physicochemical characteristics of the simple mixtures (macauba pulp oil and fully hydrogenated macaúba almond oil) that gave rise to them, without the presence of acids. trans fatty acids, banned in several countries around the world and in Brazil, with a total ban until the beginning of 2023 through RDC 332/2019 published by Anvisa.

[60] During the interesterification process, there is a random redistribution of fatty acids in the glycerol molecule, causing changes in the triacylglycerol composition, in the solids profile, etc.

[61] Chemical interesterification of mixtures of liquid oils with fully hydrogenated vegetable oils has established itself as the main alternative for the production of fats with specific functional properties.

[62] As the action of free fatty acids and peroxides as catalyst ''poisons'' is known, a specific value of sodium methoxide was used for each sample to ensure the effectiveness of the process.

Example of Concretization Raw materials and interesterification

[63] The interesterification reaction of crude macauba pulp oil (MPO) and fully hydrogenated macauba kernel oil (FHMKO) was carried out with Sodium Methoxide Catalyst powder, 99%.

Refining and hydrogenation conditions

• - Degomagem: adição de ácido cítrico;
• - Clarificação: adição de Tonsil Supreme 1800FF Clariant;
• - Desodorização/Destilação: Temperatura de 230°C, por 8 horas sob vácuo de 3 a 5 mbar.

[64] In order to increase the final quality of the oil and the efficiency of the lipid modification processes, the macaúba pulp oil was subjected to physical refining comprising the following steps:

• - Degumming: addition of citric acid;
• - Clarification: addition of Tonsil Supreme 1800FF Clariant;
• - Deodorization/Distillation: Temperature of 230°C, for 8 hours under vacuum of 3 to 5 mbar.

• - Pressão: 8kg;
• - Catalisador: 0,15% de níquel;
• - Temperatura: 180°C a 250°C;
• - Tempo aproximado de reação: 5 horas.

[65] Almond oil was subjected to a total hydrogenation process in order to obtain trisaturated fats with a high melting point and absence of trans fatty acids under the following conditions:

• - Pressure: 8kg;
• - Catalyst: 0.15% nickel;
• - Temperature: 180°C to 250°C;
• - Approximate reaction time: 5 hours.

Chemical interesterification assays of macaúba pulp oil and macaúba kernel hardfat

[66] Interesterification is performed according to the methodology of Grimaldi et al., (2005) in which 100g of the simple mixture is coupled to a vacuum system on a heating plate with agitation (20 minutes at 95°C) to the removal of moisture. Free fatty acids and peroxide act as a poison for the reaction catalyst and therefore each formulation receives a different percentage. After the formation of the "slurry", sodium methoxide is added to the lipid phase and under vacuum, the temperature is raised to 100°C for 20 minutes. Subsequently, 0.1% of 5% citric acid is added and the step of washing the interesterified formulation begins using hot water and proving the removal of soaps through the use of phenolphthalein. Finally, the formulation is heated at 110°C for 20 minutes with stirring and under vacuum to remove moisture.

[67] Table 1 shows the percentage of sodium methoxide used for each formulation. The calculation of the catalyst concentration took into account the acidity and peroxide index, acting as catalyst poison, of each formulation according to the company Desmet Ballestra (2014) represented in Table 2.

Characterization of simple and chemically interesterified mixtures

[68] Simple and interesterified mixtures are characterized by fatty acid composition, triacylglycerol composition, solid fat content, crystallization isotherm, Avrami exponent, thermal behavior through DSC, polymorphism, microstructure, consistency and rheological parameters.

Characterization of raw materials and their formulations

[69] The analytical methodologies followed the protocols and conditions recommended by the official methods of the American Oil Chemists' Society - AOCS (2009) and methodologies consolidated in the scientific literature on the characterization of lipid bases. The analytical techniques and instrumental methodology are presented below, according to the characterization of raw materials and lipid bases. These analyzes were applied to MPO and FHMKO and their formulations before and after the interesterification reaction in the established proportions.

[70] MPO and HFMKO were evaluated for free fatty acid content (%FFA), peroxide index (IP), iodine index (II), saponification index, fatty acid composition, triacylglycerol composition, Fat content solid (SFC), Isotherm of crystallization, Thermal behavior, the polymorphic form of fat crystals, Determination of microstructure and Rheology.

Solid fat content (SFC - Solid fat content)

[71] The solid fat content is a parameter used to indicate the percentage of fat that is in the solid state at a given temperature and is considered responsible for many characteristics of products such as margarines and shortenings, including spreadability, oil exudation, appearance general, ease of filling and organoleptic properties, helping in the development of formulations and consequently new products (CHIU, GIOEILLI, 2002; DIAN, SUNDRAM, IDRIS, 2007; LEE, AKOH, LEE; 2008).

[72] After the chemical interesterification reaction of FHMKO (F100) from a lauric source, there was a decrease in the solids content from 25oC, indicating that the hardfat became softer due to the increase of trisaturated triacylglycerols C42 to C48 and reduction of C52 and C54. Ramli et al (2005) analyzed the SFC of palm kernel hardfat, also from a lauric source, which showed a decrease in solids content from 15oC after randomization. The authors found that, in the same temperature range, the slope of the curve decreased and according to Timms (1979) the change in slope was probably caused by the existence of a wide variation of triacylglycerols as a result of interesterification. As FHMKO (F100 Formulation) has triacylglycerols with longer chain fatty acids compared to palm kernel hardfat, it is to be expected that the temperature at which the solids content of almond hardfat decreases (25oC) is higher than that of palm kernel hardfat. palm kernel hardfat. The SFC analysis was not applied to macaúba pulp oil, liquid at room temperature. However, Nunes et al (2015) analyzed the refined macaúba pulp oil, which presented SFC of 6.1% up to 10oC, with no remaining solids above this temperature.

[73] The effect of chemical interesterification can be noticed in all fractions, mainly from 20oC, due to the decrease of TAGs of higher molecular weight (C50 to C54) and increase of TAGs of intermediate molecular weight (C40 to C48).

[74] Figures 1 and 2 compare all formulations before and after the interesterification reaction for solid fat content. It is verified that, before the chemical reaction, the formulations show a significant decrease in the percentage of SFC from 20oC onwards, longer curves and at 60oC they were liquid.

[75] After the chemical reaction, the formulations showed a change in the curve, explained by the presence of FHMKO from a lauric source vegetable oil, a decrease in %SFC from 20oC and they were liquid at 40oC, except for the F80 formulations, F90 and F100, which had complete fusion at 45oC, further explained by the presence of higher molecular weight TAGs.

[76] According to the literature, SFC lower than 32% at 10oC has good spreadability at refrigeration temperature. The SFC at 20oC to 22oC suggests the stability of the product and its resistance to oil exudation at room temperature. Solids contents between 35oC and 37oC indicate the properties of density and flavor of fat in the mouth. Margarines that do not have a waxy mouthfeel have 3.5% SFC at 33.3oC and melt completely at body temperature (KARABULT; TURAN, ERGIN, 2004; WASSEL, YOUNG, 2007).

[77] In this context, the formulations studied do not show good spreadability at refrigeration temperature, as they present at least 40% SFC at 10oC, which could make their isolated application in creamy margarine unfeasible. Between 20oC and 30oC, the temperature range in which most of the handling of fatty products takes place, it is essential that there is no expressive reduction of solids; or that at 30oC the formulations present 15% solids due to oil exudation, characteristic behavior of plastic fats, in which the F70d and F80d formulations fit. Low solids formulations at 30oC could be indicated as fat alternatives to cocoa butter (F40d, F50d, F60d). The F90 and F100 formulations can be considered as possible substitutes for cocoa butter (CBS). All these statements need to be confirmed in the aforementioned products.

2) Melting point

[78] Table 3 shows the comparison of the melting point (oC) in the formulations before and after the lipid modification process by percentage of SFC.

[79] Melting point is defined as the temperature at which oils and fats have 4% solid fat. This value in oils and fats varies with the fatty acid chain length, degree of unsaturation due to the presence of double bonds, trans fatty acid content and fatty acid position in glycerol (KARABULUT et al., 2004). The melting points of the formulations before the interesterification reaction varied according to the interactions that occurred between the components of the raw materials, demonstrating that the mixture between oils and fats does not cause major changes when compared to the effect of interesterification (CHIU; GOIELLI; GRIMALDI, 2008). While the mixtures before the interesterification reaction showed an increase in melting point proportional to the addition of the FHMKO concentration due to the increase in the SSS content, the formulations after the random reaction showed a lower melting point, justified by the formation of new triacylglycerols of weight molecular intermediate and increased SSU content that have an intermediate melting point. Interesterified mixtures that have a melting point lower than body temperature can be applied directly to foods, as they melt completely when in contact with the mouth and do not produce a waxy sensation during consumption (GHOTRA et al. , 2002; KARABULT et al. ., 2004). The formulations that have a melting point higher than body temperature are within the range of production of solid and semi-solid fats, used mainly in confectionery and bakery products whose representative melting point is 42oC (RIBEIRO, 2009d). Although not decisive, the melting point is fundamental and is directly related to applicability.

3) Crystallization kinetics

[80] Crystallization kinetics is a parameter used to verify the crystal nucleation and growth mechanism and is related to the plasticity and rheological properties of fats (GARCIA et al., 2015). Through the crystallization isotherm, the crystallization induction time (tSFC), the crystallization half-life time (t1/2SFCmax) is obtained, which corresponds to the time required for the sample to reach half of the total solids in the stabilization and the maximum solids content (SFCmax) (CAMPOS, 2005; RIBEIRO et al., 2009a). Table 4 shows the results obtained for the formulations before and after the interesterification process.

[81] SFCmax increased with increasing FHMKO concentration. Regarding the parameters evaluated (tSFC, SFCmax and t1/2SFCmax) we observed the following aspects after the chemical interesterification reaction: increase in tSFC, decrease in SFCmax and increase in t1/2SFCmax for all formulations, due to the reduction of TAGs C50 to C54 with a consequent increase in C40, C42, C44, C46 and C48 TAGs with lower melting points.

[82] In Figures 3 and 4 it is possible to compare the solid fat content (%) as a function of time (min) of the formulations before (a) and after (d) the interesterification reaction.

microstructure

[83] The way in which oils and fats crystallize has implications for the industrial processing of formulations in which the physical characteristics largely depend on fat crystals, such as chocolates, margarines and shortenings. When the crystallization temperature is far from the melting point of the fat, smaller and more crystals are formed. Close to the melting point, the fat has a lower solid fat content and the crystals, if formed, are small and do not have specific shapes. In general, an intermediate crystallization temperature helps in the formation of larger crystals, in smaller numbers and with different shapes (SILVA, ESCOBEDO, GIOEILLI, 2008). Table 5 presents the microstructure parameters of the lipid formulations before and after the chemical interesterification reaction under stabilization at 25oC.

[84] The average diameter of the crystals of all formulations presented values lower than 30μm, considered the limit value for the fat crystal to be sensorially perceptible when the fat is applied alone (HERRERA; ROCHA, 1996).

4) Consistency

*Análise realizada em quintuplicata[85] In research on the application of lipid bases in foods, consistency analysis is one of the most important ways of evaluating functionality, as its results guide the use of fat fractions at different temperatures, classifying them according to their softness characteristics. and spreadability. According to Haighton's (1959) official methodology, consistency results are evaluated according to the Yield Value (YV) parameter according to the following classification in relation to fatty bases: YV less than 50 gF/cm2: very soft and almost fluid; YV between 50 to 100 gF/cm2: very soft and non-spreadable; YV between 100 to 200 gF/cm2: soft but spreadable; YV between 200 to 800 gF/cm2: plastic and spreadable; YV between 800 to 1000 gF/cm2: hard but satisfactorily spreadable; YV between 100 to 1500 gF/cm2: very hard with limited spreadability; YV greater than 1500 gF/cm2: very hard. Table 6 and Figures 5, 6, 7 and 8 present the YV results for the formulations before and after the interesterification reaction at three different analysis temperatures. The temperatures of 15, 25 and 35oC used to obtain the consistency results simulate, respectively, the refrigeration, ambient and thermal resistance temperatures.

*Analysis performed in quintuplicate

[86] In general, it is observed that all the simple and interesterified formulations were classified as extremely hard at 15oC, as the higher melting point TAGs were crystallized, forming a more compact and consequently harder crystal lattice, making their isolated application difficult. in food.

[87] At the temperature of 25oC, it is observed that the formulations F40, F50, F60, F70 and F80 presented, after the interesterification reaction, a lower Yield Value compared to their respective formulations before the chemical reaction, since the reduction of SSS and SSU triacylglycerols and consequent formation of intermediate molecular weight triacylglycerols resulted in smoother formulations. However, the interesterified F90 formulation showed the opposite behavior, ie, a higher Yield Value compared to its respective formulation before the interesterification reaction, due to the reduction of UUU triacylglycerols and increase of SSU. In this context, the formulations F40 and F50 before and after the interesterification reaction showed the behavior of plastic and spreadable lipid bases; and formulation F60 before and after the reaction exhibited behavior of hard bases, but satisfactorily spreadable and formulations F70, F80 and F90 did not present adequate behavior for application, as they were classified as very hard at this temperature.

[88] At 35oC, it was not possible to analyze sample F40 after the chemical reaction, which proved to be liquid at this temperature, making it impossible to obtain results. Formulations F50, F60, F70, F80 and F90 showed lower Yield Value after the lipid modification reaction compared to the respective initial Yield Value values, because at this temperature, partial crystallization of the TAGs occurred and, therefore, the crystal lattice was not fully formed and consequently results in fats with less consistency. It can be seen that at all analyzed temperatures, the Yield Value increased as the concentration of FHMKO increased, due to the presence of TAG of the SSS and SSU types in greater quantity. In this context, the formulations F40a, F50a, F60a, F70a, F80a and F90a showed behavior of plastic and spreadable fatty bases; while the F50d formulation was rated as very soft and almost fluid. Formulations F60d, F70d and F80d were rated respectively as very soft and non-spreadable, soft but already spreadable and hard but spreadable satisfactorily. On the other hand, the F90d formulation was classified as a plastic and spreadable lipid base. Finally, the F90 formulation was rated very hard, even at 35°C.

[89] At all temperatures analyzed (15oC, 25oC and 35oC), FHMKO was classified as very hard justified by its high content of SSS and SUS both before and after randomization. Through the classifications and YV obtained, it is possible, in Table 7, to observe the applications of the formulations after the interesterification reaction in products that use fats as an ingredient.

[90] In this scenario, it was possible to correlate the use of interesterified formulations from soft cake shortenings that require a lower YV to margarine or shortening puff pastry that require a high YV. In this analysis are figures 5, 6, 7 and 8.

Claims (11)

Lipid composition characterized by being based on refined macaúba pulp oil (MPO) and fully hydrogenated macaúba almond oil (FHMKO) and comprising:
- 40% to 100% FHMKO;
- 0% to 60% of MPO;
- 0.36% to 0.94% sodium methoxide;
- Solid fat content:

• - 15 to 72% SFC at 20 oC;
• - 8 to 56% SFC at 25 oC;
• - 4 to 38% SFC at 30°C

- Melting point: 30 and 41 °C;
- Crystallization kinetics:

• - tSFC: 5 to 10 minutes;
• - SFCmax: 12.75 to 60.41%;
• - t1/2SFCmax: 15 to 22 minutes;

- Consistency (Yield Value (YV)):

• - at 15°C: 1938.79 to 25546.10 gF/cm 2 ; and
• - at 25°C: 644.04 to 14976.87 gF/cm 2 ; and
• - at 35°C: 0 to 1877, 81 gF/cm 2 .

Lipid formulation characterized by comprising 40% FHMKO, 60% MPO, 0.58 sodium methoxide and the characteristics:
- Solid fat content:

• - 15% SFC at 20°C;
• - 8% SFC at 25 oC;
• - 4% SFC at 30°C;

- Melting point: 30 oC;
- Crystallization kinetics:

• - tSFC: 10 minutes;
• - SFCmax: 12.75%;
• - t1/2SFCmax: 22 minutes;

- Consistency (Yield Value (YV)):

• - at 15°C: 3191.63 gF/cm 2 ; and
• - at 25 oC: 644.04 gF/cm2.

Lipid formulation characterized by comprising 50% FHMKO, 50% MPO, 0.65 sodium methoxide and the characteristics:
- Solid fat content:

• - 25% SFC at 20°C;
• - 12% SFC at 25°C;
• - 6% SFC at 30°C
• - Melting point: 33 °C;

- Crystallization kinetics:

• - tSFC: 9 minutes;
• - SFCmax: 19.74%;
• - t1/2SFCmax: 18 minutes;

- Consistency (Yield Value (YV)):

• - at 15°C: 1938.79 gF/cm 2 ;
• - at 25°C: 268.57 gF/cm 2 ; and
• - at 35°C: 35.36 gF/cm 2 .

Lipid formulation characterized by comprising 60% FHMKO, 40% MPO, 0.70 sodium methoxide and the characteristics:
- Solid fat content:

• - 33% SFC at 20°C;
• - 20% SFC at 25°C;
• - 10% SFC at 30°C
• - Melting point: 35 °C;

- Crystallization kinetics:

• - tSFC: 7 minutes;
• - SFCmax: 26.53%;
• - t1/2SFCmax: 19 minutes;

- Consistency (Yield Value (YV)):

• - at 15°C: 3071.76 gF/cm 2 ;
• - at 25°C: 1058.21 gF/cm 2 ; and
• - at 35°C: 82.81 gF/cm 2 .

Lipid formulation characterized by comprising 70% FHMKO, 30% MPO, 0.76 sodium methoxide and the characteristics:
- Solid fat content:

• - 42% SFC at 20°C;
• - 28% SFC at 25°C;
• - 15% SFC at 30°C
• - Melting point: 37.5 °C

- Crystallization kinetics:

• - tSFC: 7 min;
• - SFCmax: 34.00%;
• - t1/2SFCmax: 16 min;

- Consistency (Yield Value (YV)):

• - at 15°C: 4108.16 gF/cm 2 ;
• - at 25°C: 1554.59 gF/cm 2 ; and
• - at 35°C: 146.97 gF/cm 2 .

Lipid formulation characterized by comprising 80% FHMKO, 20% MPO, 0.82 sodium methoxide and the characteristics:
- Solid fat content:

• - 53% SFC at 20°C;
• - 38% SFC at 25°C;
• - 20% SFC at 30°C

- Melting point: 39 °C;
- Crystallization kinetics:

• - tSFC: 7 minutes;
• - SFCmax: 47.52%;
• - t1/2SFCmax: 16 minutes;

- Consistency (Yield Value (YV)):

• - at 15°C: 4900, 09 gF/cm 2 ;
• - at 25°C: 22 57.25 gF/cm 2 ; and
• - at 35°C: 263, 17 gF/cm 2 .

Lipid formulation characterized by comprising 90% FHMKO, 10% MPO, 0.88 sodium methoxide and the characteristics:
- Solid fat content:

• - 62% SFC at 20°C;
• - 46% SFC at 25°C;
• - 25% SFC at 30°C

- - Melting point: 40 °C;
- Crystallization kinetics:

• - tSFC: 6 minutes;
• - SFCmax: 49.81%;
• - t1/2SFCmax: 15 minutes;

- Consistency (Yield Value (YV)):

• - at 15°C: 6631.17 gF/cm 2 ;
• - at 25°C: 37 68.16 gF/cm 2 ; and
• - at 35°C: 391.05 gF/cm 2 .

Lipid formulation characterized by comprising 100% FHMKO, 0.36 sodium methoxide and the characteristics: - Solid fat content:

• - 72% SFC at 20 oC;
• - 56% SFC at 25°C;
• - 38% SFC at 30°C;

- Melting point: 41 °C;
- Crystallization kinetics:

• - tSFC: 5 minutes;
• - SFCmax: 60.41%;
• - t1/2SFCmax: 15 minutes;

- Consistency (Yield Value (YV)):

• - at 15°C: 25546, 10 gF/cm 2 ;
• - at 25°C: 14976, 87 gF/cm 2 ; and
• - at 35°C: 1877, 81 gF/cm 2 .

Use of the lipid composition as described in claim 1, characterized in that it is applicable in masses in general such as cookies, breads and cakes, stuffed cookies, fillings, light creams, margarines, candies, chocolate toppings, cocoa butter substitutes (CBS), toppings for ice cream, among others. Use of lipid formulations as described in claim 2, 3, 4, 5, characterized in that it is applicable to pasta in general such as cookies, breads and cakes, stuffed cookies, fillings, light creams, margarines, candies, among others. Use of lipid formulations as described in claims 6, 7 and 8, characterized by being applicable in chocolate toppings, cocoa butter substitutes (CBS), toppings for ice cream.

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