MXPA99009643A - The production of a food acid mixture containing fumaric acid - Google Patents

Abstract

A method for the production of a food acid includes the steps of combining fumaric acid with an organic acidic material in an aqueous medium to produce a mixture and drying the mixture to produce a food acid comprising a particulate material containing fumaric acid and the organic acidic material, the quantity of fumaric acid and the quantity of the organic acidic material being selected so that the fumaric acid makes up between about 5%and 95%of the particulate material.

Description

METHOD TO PRODUCE A MIXTURE OF FOODSTUFFS CONTAINING PHYNARIC ACID AND THE PRODUCT OBTAINED DESCRIPTION OF THE INVENTION This invention relates to a method for the production of a food acid and to a food acid produced according to the method. US-A-3, 506, 453 discloses agglomerated fumaric acid compositions prepared by mixing finely divided components with a liquid amount barely sufficient to cause the surface of the component to become tacky. The components are then contracted with a moist air stream and the components agglomerate to form a porous agglomerated product. According to a first aspect of the invention, there is provided a method for the production of a food acid, the method includes the steps of combining fumaric acid with an organic acid material that is selected from malic acid, tartaric acid, citric acid, lactic acid, ascorbic acid and mixtures of any two or more thereof in an aqueous medium to produce a mixture; and drying the mixture to produce a food acid comprising a particulate material containing fumaric acid and the organic acid material, the amount of fumaric acid and the amounts of the organic acid material are selected such that the fumaric acid constitutes between 5% and 95% of the particulate material, the combining step is selected from one of mixing finely divided fumaric acid with an aqueous solution of the organic acid material; grinding the fumaric acid in the presence of an aqueous solution of the organic acid material to produce a suspension; and triturating the fumaric acid in an aqueous medium to produce a milled suspension of fumaric acid and then adding the organic acid material to the milled suspension of fumaric acid. The percentages in the compositions that are provided in this specification refer to the percentages of composition by mass. Preferably, the amount of fumaric acid and the amount of the organic acid material will be selected such that the fumaric acid constitutes between about 40 and 60% of the particulate material, and more preferably between about 45 and 55%. The fumaric acid can be fumaric acid soluble in cold water (or C S). Cold water soluble fumaric acid refers to finely ground fumaric acid which includes a small amount of a wetting agent of the type sold as CWS fumaric acid by Haarman and Rei er or a granular fumaric acid material of the type sold by NCP Food Products such as granular cold water soluble fumaric acid.

The organic acid material can be selected from malic acid, tartaric acid, citric acid, lactic acid, ascorbic acid and mixtures of any two or more thereof. Preferably, the organic acid material will be a mixture of malic acid and tartaric acid. Organic acids are therefore edible acids soluble in water, that is, acids allowed in food. The amount of malic acid can be selected such that the malic acid constitutes up to about 40-60% of the particulate material, and preferably about 50%. The amount of tartaric acid can be selected such that the tartaric acid constitutes about 3-10% of the particulate material and preferably about 5%. The method may therefore involve mixing finely divided fumaric acid with an aqueous solution of malic acid and tartaric acid. The mixing step may include grinding the fumaric acid in the presence of an aqueous solution of the malic acid and tartaric acid to provide a suspension or grinding of fumaric acid in the aqueous medium and then adding or combining the malic acid and the tartaric acid in the aqueous medium. suspension of ground fumaric acid or spray the aqueous solution of malic acid and tartaric acid or spray separate solutions of malic acid and tartaric acid on fumaric acid in powder form.

Therefore, the combination step can include mixing finely divided fumaric acid with an aqueous solution of malic acid and tartaric acid. Instead, the combination step can include grinding the fumaric acid in the presence of an aqueous solution of malic acid and tartaric acid to produce a suspension. Instead, the combination step can include grinding the fumaric acid in an aqueous medium to produce a milled suspension of fumaric acid and then adding or combining the malic acid and the tartaric acid within the milled suspension of tartaric acid. Instead, the combination step may include spraying an aqueous solution of malic acid and tartaric acid over fumaric acid in powder form. Instead, the combination step may include spraying separate aqueous solutions of malic acid and tartaric acid onto fumaric acid in powder form. The grinding step can be carried out in a wet mill so that the mixture is in the form of a suspension in which the particle size of essentially all of the solid material in the suspension is not more than 150 microns (mesh) 100) and the average particle size is between approximately 100 and 25 micrometers (150-500 mesh). Preferably the grinding step is carried out so that the particle size of essentially all of the solid material in the suspension is not more than 100 microns (150 mesh) and the average particle size is between about 75 and 25 microns ( 200-500 mesh). The drying step may include spray drying or spray granulation of the suspension. Therefore, the drying step can be selected from spray drying and spray granulation. In particular, the drying step can be a spray granulation step which is carried out in a fluid bed granulator by a continuous process or in batches to provide a free flowing product that does not generate dust. The spray granulation step can be controlled so as to directly produce 20-60 mesh granules, preferably 30-45 mesh granules, or those selected from the product by sieving, where the rejected material can be reprocessed. The final particle size is typically controlled by sieving or sifting, to remove larger sized particles which are then ground finely in a mill and returned to the fluidized bed of the granulator. The undersized particles are also removed by sieving or sifting and then returned to the fluidized bed. In addition, when the drying step is carried out by a continuous process, a certain amount of material segregation of the particles takes place as the smaller particles are raised higher and tend to come into contact with fresh solution / suspension which is sprayed in the bed, and consequently grow in preference to the larger particles, which remain in the lower bed extensions. The overflow of the bed is usually located near the bottom of the bed to remove the larger particles. In this way, the final particle size is controlled between approximately 20 and 100 mesh (840-150 micrometers) and ideally between approximately 24 and 60 mesh (700-250 micrometers). After the spray granulation step, the particulate material can be dried to a moisture level of less than 0.5% and preferably less than 0.25%. Therefore, the mixture can be dried to produce a particulate material having a moisture level less than 0.5%, and preferably less than 0.25%. The combining step can be carried out in the presence of a wetting or surfactant agent. The wetting agent can be dissolved, for example, in an aqueous medium so that the particulate material which is produced is uniformly mixed with the wetting agent. further, the mixing step can be carried out in the presence of an antifoam agent. The antifoaming agent can also be dissolved in the aqueous solution. The wetting agent can be a liquid wetting agent. Such liquid wetting agent will typically be edible and essentially tasteless. For example, it may be a liquid alkyl sulfosuccinate such as dioctylsodium sulfosuccinate, sodium lauryl sulfite, Tween (trade name) or any other edible wetting agent or surfactant. The antifoaming agent can be a silicone antifoaming agent. It can be, for example, a food grade silicone oil antifoaming agent. The amount of the wetting agent can be selected such that it constitutes approximately 0.1-0.5% of the final product, ie, the food acid. The amount of the antifoaming agent can be selected so as to control the foam during the mixing and drying steps and to constitute about 2-20 ppm, preferably about 5-15 ppm, and much more preferably about 10 ppm of the product final, that is, the food acid. The method may include the additional step of incorporating an additive that is selected from flavors, colorants, sweeteners and mixtures of two or more thereof in the food acid. Typically, the additive will be sprayed onto the mixture during the spray drying or spray granulation stage. The invention extends to a food acid in particulate form produced by the methods described in the present invention. The invention further extends to a food acid in particulate form, the food acid comprises a composite material which includes fumaric acid in an amount of about 5% -95%, malic acid in an amount of about 5-95% and tartaric acid in an amount of about 3-15%. The invention is now described, by way of example, with reference to the accompanying examples and figures, in which the words "compound acid" and "compound" refer to the food acid of the invention. In the figures: figure 1 shows the expected acid profile of the compound acid; Figure 2 shows the acid profile of citric acid; Figure 3 shows the acid profile of malic acid; Figure 4 shows the acid profile of fumaric acid; Figure 5 shows the acid profile of tartaric acid; Figure 6 shows an overlap of the acid profiles of Figures 1 to 5 and the expected acid profile of the compound acid; Figure 7 shows the adsorption isotherms of the compound and the citric acid; and Figure 8 shows the pH profiles of the compound and citric acid.

EXAMPLE 1 Malic acid (40 kg), dl-tartaric acid (4 kg) and dioctyl sulfosuccinate wetting agent (Zenith DSS, 100 g) are dissolved in hot water (130 kg) to produce a solution. Crystalline fumaric acid (36 kg) is added to the solution, and the resulting suspension is milled in a Chicago Boiler rubbing mill for two hours. In the other modalities, the mill is a supermolino EHP series provided by Premier Mili or Oliver and Battle. A silicone antifoaming agent (AF 1510, supplied by Bob Larson Silicones, five drops) is used to control the foaming during the grinding process. A crystalline tartaric acid initiator bed (200 g) is added to the GLATT GPCG-60 batch spray granulator adapted with a triple spray nozzle and the milled suspension is sprayed on the starter bed at 70-130 1 / h for 130 minutes so that the temperature in the fluidized bed is maintained at 50-60 ° C. The mill is a 22 kW unit which has a height of approximately 1300 mm with a diameter of approximately 800 mm and a tip speed in the impeller of 13 m / s. The settings of the granulator were: spray air pressure 2.5 bar air inlet temperature 100 ° C air flow 2200 m3 / h.

The product is then dried by further fluidization for 30 minutes and cooled by fluidization for 5 minutes in cold air to a bed temperature of 40 ° C.

EXAMPLE 2 Example 1 is repeated using water (60 kg) and a starter bed of the product of example 1 (10 kg). The temperature of the bed during the granulation process is maintained at 52-57 ° C. The product contains 0.21% water by mass and 81.4% by mass is in the size range of 841-250 micrometers. The bulk density is 690-774 kg / m3. The acid taste profile of the granular product produced by the method of example 1 is set forth in figure 1.

EXAMPLE 3 The following food grade ingredients were added to a mixed mixing container fitted with a stirrer at the indicated rates, and mixed: Tartaric acid 50 kg / hour Malic acid 500 kg / hour Fumaric acid 450 kg / hour wetting agent dioctyl sulfosuccinate (70%) 2.25 kg / hour Silicone oil antifoam 15 g / hour Water 500 1 / hour The mixing vessel has a capacity of about 1500 1 and is large enough to allow adequate mixing and time for the soluble ingredients to dissolve. Only the fumaric acid did not dissolve, so that a suspension formed. The suspension is continuously fed into a wet Mill of the Premier type in which it is milled. The ground slurry is then pumped directly under pressure to an APV Anhydro continuous drying / granulating unit using a positive displacement pump where the granulation and initial drying of most of the moisture (decreasing to approximately 1% residual) takes place in a fluidized bed in the first stage of the unit. The first stage comprises a generally round oblate container, into which the suspension is pumped continuously under pressure through a nozzle in a fluid bed. This process can be carried out optionally with or without atomization by compressed air. The fluid bed is suspended above the screen plate by a stream of hot air. The bed is fluidized with hot air at about 65 ° C at surface speeds used in fixed fluid tanks, which typically are in the range of 0.3-2.4 m / s. The height of the bed is controlled by the volume and pressure of the air entering the chamber from the bottom of the screen, while the volume and time of residence of the product in the fluid bed are maintained under the conditions established by allowing a certain quantity leaves the bed through a rotary outlet valve, and enters a second stage. The air outlet from the first chamber is passed through the upper part of the container through a cyclone to move the entrained product fines which return to the fluidized bed where they are contacted with the incoming aspersion and with other particles in the bed. This helps regulate the particle size range of the product by cooling the fines to the bed to grow to larger granules. The second stage consists of a rectangular fluid bed that vibrates mechanically or optionally a stationary fluid bed, at a slight angle, where the product moves forward by air flows, where additional drying and subsequent cooling take place. Both air currents, hot and cold, are collected with the fines that were removed by the cyclone and returned to the fluid bed of the first chamber. Additional additives such as flavorings, colorants and / or sweeteners can optionally be incorporated by spraying the additive into the granules in the second step. The dry and cooled product of the second stage, which has a low residual moisture content of typically less than 0.3%, is subjected to overflow to a landfill which maintains a predetermined residence time, on a screen in which the particles are removed. larger size and crushed before they return to the fluid bed of the first stage, along with the smaller sized fines which are separated by sieving. The sieving machine controls the final particle size of the product, while the extraction ducts from the top of the second stage unit further classify the product by extracting fines and dust which has been removed from the airstream. by the cyclone and return to the fluid bed of the granulator of the first stage.

DISCUSSION Food acids are generally used to provide a refreshing and pleasant acid taste to foods, liquids and beverages. They also serve as preservation • aids by lowering the pH of the food product to which they are added so they reduce the activity of potentially harmful microorganisms. For many years citric acid has been used for this purpose.

The acid flavor profile of citric acid, as set forth in Figure 2, can be described as a rapid "discharge" of acidity which reaches a maximum acid taste very soon, then the flavor diminishes and disappears very quickly thereafter. The sharp and sharp acid taste of citric acid, however, tends to exacerbate the taste of sweeteners and flavorings in a food product to which citric acid has been added. The relatively rapid loss of acidity results in a bitter aftertaste if certain high intensity synthetic sweeteners are used in the food product together with the citric acid. The citric acid suffers from the additional disadvantages besides that it is a strong sharp flavor, of a short-lived acid flavor. For example, when used in dry powders, such as non-alcoholic beverages and beverage mixes, it tends to sediment due to its hygroscopic nature. In addition, it generally does not flow freely and has a particle size that is not uniform. Despite these drawbacks, citric acid is the acidulant most commonly used in food. Malic acid, which is soluble like citric acid, has an acidic flavor profile as shown in Figure 3. The flavor profile is described not as sharp as citric acid, but with a longer duration. Therefore, malic acid tends to mask the bitter aftertaste of the synthetic sweeteners used together with malic acid. The slower increase in peak acidity does not exacerbate the taste of sweeteners with the result that less sweetener needs to be used (this has been found to be the case with aspartame). In taste tests, it has been claimed that flavorings are more effectively fused with malic acid. However, the initial discharge associated with citric acid is preferable in some final products such as citrus flavored beverages. The fumaric acid has an acid profile which is flatter than that of citric acid or malic acid but has a longer duration, as can be seen in figure 4. A flavor that lasts longer means that fumaric acid appears effectively as a "stronger" food acid and consequently less fumaric acid is required to reach the required level of acidity compared to that required for other food acids. However, although fumaric acid is generally one of the cheapest food acids, it has little solubility in water and a tendency to slowly dissolve unless it is supplied, for example, in a very fine powder that includes a wetting agent, ie , those which are called soluble in cold water or fumaric acid CWS of the type described above or soluble fumaric acid in cold granular water as described above. All other cold water soluble fumaric acids known to the applicants are very dusty and therefore are not suitable for many applications. The acidity profile of di or 1 tartaric acid can be seen in Figure 5 is more uniform than that of citric acid. It has a maximum acid taste which is greater than that of citric acid and with a longer duration. Tartaric acid is usually the most expensive of commonly used food acids. However, the isomer of 1-tartaric acid is hygroscopic and consequently tends to sediment. The sensory profiles of acidity established in figures 1 to 5 are obtained from the literature. A typical method for determining these profiles is based on a TASTE software package (See 9.1, 1992) developed by Reading Scientific Services Limited, The Lord Zuckerman Research Center, The University of Whiteknights, READING, UNITED KINGDOM. In order to obtain a point of equiabic flavor of the acidic compound in relation to the citric acid monohydrate, a team of tasters is prepared and trained. Equiated concentrations are the concentrations of food acids in which there is an equal perception of acidity and an acidity for the taste. The analysis consists of the testing by the tasting team of the four basic tastes (sweet, sour, salty and bitter) and several sets of concentration series to determine the threshold value of the group, according to Jellineck, 1985. triangular tests to determine the threshold value of each member of the tasting team for each basic flavor according to the ASTM standards. Subsequently, the twelve members most sensitive to bitter taste were selected as part of the panel of acid tests. The sets of concentration series used in the training were used as an indication of the range of the series of concentrations to be used in the equia- test test. CSIR supplies the set of series of concentrations for the analysis of equiated flavor. If the series is too low or too high to cover the range in which the acid taste point of citric acid is found, a higher or lower series is requested and used. The most applicable series with a range of five concentration levels were repeated at least three times. The concentration of citric acid was 0.2%. Samples are presented in random ordered pairs with 0.2% citric acid, in ascending order of concentration, with two pairs per session, with an interval of 20 minutes between sessions to avoid sensorial fatigue of the taster team. Instant flan with a cleanser between the sessions is used. All samples, water and flan were served at room temperature (19.4 - 22.3 ° C). The samples were tested in individual cabinets for taste tests with controlled temperature under normal white light.

The results obtained were analyzed statistically by the ARC-Agrimetrics Institute, using Genstat 5, version 3.1 (1993). The equiac concentrations were as follows: The above clearly shows savings in use. The concentrations reflect a saving of 37.5% compared to citric acid monohydrate and a saving of 33.5% when compared to anhydrous citric acid. These savings vary based on the taste characteristics of the product. These tests were followed by a comparison of the flavor characteristics of the citric acid and the acid compound. The panel was trained using acidic test solutions at an equidiated taste point, and products similar to acetic acid, unripened bananas, cold black tea and various snacks and 'non-alcoholic beverages. This training introduced the panelists to possible typical descriptive terms for acids. The attributes shown in table 1 were generated and defined by the taster team during the training sessions. The samples were presented in the same procedure as above. The statistical analysis was collected in a spreadsheet using Quattro Pro (V 5.0) and a statistical program, STATGRAPHICS (V 5.0) was used to analyze the data using the one-way analysis of variance (ANOVA) with the acid as the effect principal .

TABLE 1 From the results obtained it was found that there are no significant differences between any of the sensory related variables for citric acid (0.2% w / v) of the acid compound or its equiated point. Therefore, it can be concluded that a combination of these three acids in the compound acid can very closely match the acidic sensory profile of citric acid through the various attributes measured at equiated concentrations. The Applicant has found by the use of malic acid, fumaric acid and tartaric acid together, that it is possible to overcome the known disadvantages of citric acid and the individual disadvantages associated with malic, fumaric and tartaric acids, and to provide a composite granule which contains each of the acids, which have an improved acid flavor profile. It is expected that the sensory acid profile of the compound acid compared to other food acids will closely resemble that shown in Figure 6. In this manner, the invention allows the substitution of hygroscopic citric acid with a non-hygroscopic granular compound mixture of malic acid. , dl-tartaric acid (or l-tartaric acid if di tartaric acid is not allowed as food acid or if it is not available) and fumaric acid (all of these acids are food grade and non-hygroscopic in the granular form composed of present invention). The empirical data clearly indicate the hygroscopic nature of citric acid compared to the relatively non-hygroscopic properties of the compound acid when tested under control conditions for example by the sorption isotherm measurements performed by the CSIR, as can be seen in Figure 7 The small amount of tartaric acid present in the composite granules provides a sudden "discharge" of acidity similar to that of citric acid while the main portion of malic acid, which is very soluble, provides a mild acid taste. The low solubility of fumaric acid can be resolved using cold water soluble fumaric acid (CWS) and the low solubility of fumaric acid is solved by selecting the amount of fumaric acid in the composite granule so that the selected amount will be soluble in the amount of water that is used. Citric acid has only the following disadvantages. It is hygroscopic and tends to sediment. It is not free-flowing, has a non-uniform particle size, and has an excessive generation of initial acrid taste and a short-lived acid taste. further, mixtures of acids generally have a non-uniform distribution of components and the separation (stratification) of the components due to different particle size and different specific gravity occurs frequently. Such combinations also have an irregular appearance. The presence of fumaric and malic acids in the granular product also results in savings in the total amount of acidulant needed when compared to citric acid and provides a longer lasting acid taste.

TABLE 2 Average ratings for citric acid compared to the compound acid at the equiated point where, for all attributes: 1 = none; 8 Extremely One advantage of the illustrated invention is that it provides a granular solid in which each granule is a composite granule (as opposed to a composition) which contains malic acid, tartaric acid and fumaric acid and in which the granules have a size of consistent particle. The product has a good flavor reminiscent of the taste of natural fruits with a mild acidity of long duration and a uniform distribution of various acids within the granulate. A further advantage of the illustrated invention is that the granular product is free-flowing, dust-free and non-hygroscopic, and has improved handling, packing and shelf-life characteristics when compared to the acidulants of the prior art of which it is known by the applicants and, in addition, has a uniform acidity of long duration and a lower cost compared to the food acids of the prior art which are known by the applicant. The pH profile of the compound acid shows a consistently lower pH value at different concentrations than that which can be obtained by citric acid, as can be seen in Figure 8 and Table 3.

TABLE 3 pH of the compound acid and citric acid at different concentrations

Claims (22)

1. Method for the production of a food acid, the method includes the steps of combining fumaric acid with an organic acid material that is selected from malic acid, tartaric acid, citric acid, lactic acid, ascorbic acid and mixtures of two or more of the themselves in an aqueous medium to produce a mixture; and drying the mixture to produce a food acid comprising a particulate material containing fumaric acid and the organic acid material, the amount of fumaric acid and the amounts of the organic acid material are selected such that the fumaric acid constitutes between 5% and 95% of the particulate material, the combining step is selected from: mixing finely divided fumaric acid with an aqueous solution of the organic acid material; triturating the fumaric acid in the presence of an aqueous solution of the organic acid material to produce a slurry; and triturating the fumaric acid in an aqueous medium to produce a slurry of milled fumaric acid, and then adding the organic acid material to the slurry of milled fumaric acid.

2. Method as described in claim 1, wherein the amount of fumaric acid and the amount of organic acid material is selected such that the fumaric acid constitutes between 40 and 60% of the particulate material.

3. Method as described in claim 2, wherein the amount of fumaric acid and the amount of organic acid material are selected such that fumaric acid constitutes between 45 and 55% of the particulate material.

4. Method as described in any of the preceding claims, wherein the fumaric acid is fumaric acid soluble in cold water (or CWS).

5. Method as described in any of the preceding claims, wherein the organic acid material includes malic acid and the amount of malic acid is selected such that the malic acid constitutes 40-60% of the particulate material.

6. Method as described in claim 5, wherein the amount of malic acid is selected such that malic acid constitutes up to 50% of the particulate material.

7. Method as described in any of the preceding claims, wherein the organic material includes tartaric acid and the amount of tartaric acid is selected such that the tartaric acid constitutes 3-10% of the particulate material.

8. Method as described in claim 7, wherein the amount of tartaric acid is selected such that tartaric acid constitutes up to 5% of the particulate material.

9. Method as described in any of the preceding claims, wherein the step of grinding is carried out in a wet mill so that the particle size is essentially for all the solid material in the slurry no greater than 150 microns (100 mesh) and the average particle size is between 100 and 25 microns (150-500 mesh).

10. Method as described in claim 9, wherein the grinding step is carried out in a wet mill such that the particle size of essentially all the solid material in the slurry is not more than 100 microns (mesh 150) and the average particle size is between 75 and 25 microns (200-500 mesh).

11. Method as described in any of the preceding claims, wherein the drying step is selected from spray drying and spray granulation.

12. Method as described in claim 11, wherein the drying step is a step of spray granulation which is carried out in a fluid bed granulator by, a process that is selected from a continuous process and a process by charges to give a product that flows freely without dust.

13. Method as described in claim 11 or 12, wherein the spray granulation step is controlled so that the 20-60 mesh granules are produced directly.

14. Method as described in any of the preceding claims, wherein the mixture is dried to produce a particulate material having a moisture level of less than 0.5%.

15. Method as described in any of the preceding claims, wherein the mixture is dried to produce a particulate material having a moisture level less than 0.25%.

16. Method as described in any of the preceding claims, wherein the combining step is carried out in the presence of a wetting agent or surfactant.

17. Method as described in claim 16, wherein the wetting agent is dissolved in the aqueous medium such that the particulate material that is produced is uniformly mixed with the wetting agent.

18. Method as described in claim 16 or 17, wherein the wetting agent is a liquid wetting agent.

19. Method as described in claim 18, wherein the wetting agent is selected from dioctylsodium sulfosuccinate, sodium lauryl sulfate and Tween (trade name).

20. Method as described in any of the preceding claims, which includes the step of incorporating an additive that is selected from flavors, colorants, sweeteners and mixtures of any two or more thereof in the food acid.

21. A food acid in particulate form produced by the method described in any of the preceding claims. •

22. A food acid in particulate form, the food acid comprises a composite material which includes fumaric acid in an amount of about 5-95%, malic acid in an amount of about 5-95% and tartaric acid in an amount of about 3- fifteen%.