MXPA98002584A - Microgranula for food applications / forr - Google Patents

Abstract

The present invention relates to a microgranular composition of enzymes having an average particle size of from about 20 to 400 microns. The microgranular composition has characteristics of low pulverization, high miscibility and rapid dispersion, particularly beneficial for the food and feed industries. The methods for making said microgranules containing enzymes are also described.

Description

MICROGRAPH FOR APPLICATIONS IN FOOD / FORAGE Field of the Invention This invention relates to improved microgranules of enzymes, particularly useful in food and feed applications, as well as agglomeration processes for the production of said microgranules.

Background of the Invention The use of enzymes, especially of microbial origin has become more common. Enzymes are used in different industries, including but not limited to, the starch industry, the dairy industry, the detergent industry and the food or bread industry, as well as the animal feed industry. Various available products of dry enzymes are associated with potential occupational hygiene concerns, mainly in relation to the exposure of workers to airborne enzyme dust, and generally, to the dusty products of available enzymes. Various granular products useful in the food and feed industries are spray dried. These products tend to be dusty in handling.

REF: 27050 Since the introduction of enzymes in the segments of detergents and in other industrial, various developments have been made with respect to the granulation and coating of enzymes to reduce enzyme dust. However, in the current state of an increasing environmental concern, and a high awareness of industrial hygiene, there remains a continuing need for low dust enzyme granules. Moreover, there are additional desirable characteristics in enzyme granules that are not currently available in known granulation products, and particularly for enzyme granule products directed to the food and feed industries. For example, in the food industry a granular enzyme product must incorporate the starting materials (such as carriers, binders and coating materials) that are of food grade quality. Moreover, it is desirable that the granules of food enzymes are microgranular in size, in other words, that they are between 20-400 microns in size, so that the granules mix well with other food ingredients and disperse rapidly with a distribution uniform enzyme when it is present in an aqueous medium.

Therefore, it is an object of the present invention to provide low dust microgranules having a majority of particle sizes in the range of 20-400 microns. These microgranules are preferably dispersible or miscible with food ingredients (ie, baking), and rapidly disintegrate in an aqueous medium to provide rapid availability of the enzyme.

Another object of the present invention is to provide an agglomeration process using fluidized bed spray and drying technology to prepare the low dust granules of the present invention.

Brief Description of the Invention In accordance with the present invention, microgranules are provided which contain enzymes comprising: a) a suitable carrier b) an aqueous source of enzymes c) one or more binder (s) or disintegrant (s); and d) a food grade polymer coating agent, soluble in water; the microgranule has an average size between 20 and 400 microns, preferably around 20 to 200 microns.

The microgranules containing enzymes of the present invention can comprise any enzyme; however, in a preferred embodiment of the present invention, the enzyme is useful in the food and / or baking industry. Thus, useful enzymes include, but are not limited to, enzymes selected from the group consisting of proteases, amylases, cellulases, xylanases, endoglycosidases and glucose oxidases or mixtures thereof.

This invention also relates to methods for making low dust granules. One embodiment of the method of the present invention comprises: a) loading a suitable carrier into a fluid bed granulator; b) mixing an aqueous source of enzymes and one or more appropriate binders and / or disintegrating agent (s); c) atomizing the enzyme and binder mixture of step b) onto the carrier; and d) atomizing the product of step c) with a food-grade polymer soluble in water at a rate to form a coating and maintaining a particle size from about 20 to 400 microns, preferably 20 to 200 microns; with the proviso that steps a) and b) can be carried out in any order.

Detailed Description of the Invention As used herein, a "suitable carrier" means any carrier material that has physical characteristics that are similar to other ingredients used in the food / feed industry. The carrier can be insoluble or soluble in water. Thus, for example, suitable carriers (particularly for the food / bakery industry) include but are not limited to soybean meal, soybean meal, cornmeal, ground corn cobs or cellulose type material, such as powder of alpha-cellulose, normal or spray-dried lactose, maltodextrins, corn syrup solids, etc.

As used herein, "binder" means one or more material (s) that are found alone or in combination with sugars (such as sorbitol) and act to bind the enzyme to the carrier material, thereby forming agglomerates. Binders useful in the present invention include, for example, hydrolyzed starches (such as Miragel or Puré-Gel, commercially available from Staleys, GPC) and gums (such as xanthan gum or acacia sheath gum). The hydrolyzed starches may be used together with the sugars (such as corn syrup solids) as a binder and disintegrant useful in the present invention. Particularly, the starch plus the corn syrup solids in the present invention are preferred, since the combination provides a matrix for melting together the carrier particles to build the particle size, and the corn syrup solids which are hydrophilic, they help to disperse and break up the granule in the presence of an aqueous environment (such as the small amount of water used during the dough making process).

As used herein, "water soluble food grade polymer" means any food polymer soluble in water, and includes, but is not limited to, high or low viscosity algin and algin mixtures (such as Keltone ™, commercially available from Kelco ) and Gellan gum and mixtures of these.

Any enzyme or combination of enzymes can be used in the present invention. During a fluidized bed granulation process, the enzymes are typically atomized from relatively impure solutions and suspensions in which the active enzyme constitutes only a portion of the total dissolved and suspended solids. Other suspended solids present in the fermentation broth include proteins, peptides, carbohydrates, other organic molecules and salts. Preferred enzymes for the microgranules of the present invention include those enzymes useful in the food (including bakery) and fodder industries. Said enzymes include but are not limited to proteases (bacterial, fungal, acid, neutral or alkaline), amylases (alpha or beta), lipases (fungal, bacterial or mammalian), cellulases (whole cellulase or functional components thereof), xylanases and glucose oxidases and mixtures thereof. When the enzyme microgranules of the present invention are used in food applications, the enzyme must be of food grade quality. Thus, for example, suitable enzymes include cellulases, lysozymes and proteases available under the trade name Multifect from Genencor International, Inc., Rochester, NY or the glucose oxidase available under the trade name OxyGO from Genencor International, Inc., Rochester, NY.

As is known to those skilled in the art, other ingredients attached to the microgranules of enzymes of the present invention can be added. The adjunct ingredients may include: metal salts, solubilizers, activators, antioxidants, dyes, inhibitors, binders, fragrances, enzyme protective agents / scavengers such as ammonium sulfate, ammonium citrate, urea, guanidine hydrochloride, guanidine carbonate, sulfonate of guanidine, thiourea dioxide, monoethanolamine, diethanolamine, triethanolamine, amino acids such as glycine, sodium glutamate and the like, proteins such as bovine serum albumin, casein and the like, depending on the proposed final use of the microgranule.

A preferred composition of the microgranules of the present invention comprises an active ingredient of enzymes useful in the food industry, a carrier of soybean meal, a modified starch binder which is used in combination with a sugar to bind the enzyme to the carrier of Soybean meal and act as a disintegrant, and a polymer of high viscosity, soluble in water, food grade, film former.

Thus, for example, a preferred microgranule of the present invention comprises: Ingredient quantity / ioo ks cellulase concentrate (22.5% solids) 160.0 Miragel 463 2.0 Keltone ™ HV 200.0 gm corn syrup solids 8.0 kg soy flour 53.8 kg The skilled formulator will readily recognize that the amount of enzyme will be adjusted according to the desired activity for the finished product. Similarly, the amount of polymer such as Keltone ™ will vary from 0.1 to 0.3% depending on the thickness of the coating. The amount of corn syrup used, if any, will vary from 4-15% depending on the volume of enzyme fluid and the desired particle size of the finished product, and the amount of carrier (such as soy) will be adjusted based on in the activity and the solids in the enzyme concentrate.

The microgranules of the present invention have a particle size of between about 20-400μ, preferably 20-200μ. The particle size is important because particularly for the food and bakery industries, an enzyme microgranule of this particle size range will mix well with other ingredients in the food products (such as dough mixes, etc.).

In a process aspect of the present invention, the microgranules are made by agglomeration. This methodology results in low-dust products (as compared to freeze-dried or spray-dried enzyme products) and more cost-efficient production. Preferably the microgranules are prepared in a fluid bed granulator, although other equipment such as oscillating granulators or high-strength granulators can be used. A fluid bed granulator is preferred, in part because of its ease of operation of the process by which suitable binders such as sugar and hydrolyzed starch are mixed together with a liquid enzyme which is then mixed and atomized on the carrier. Two targets are reached during the atomization process: the enzyme is placed in the carrier and the particle accumulates to a granular form (within the desired size range). A suitable food grade polymer is then atomized onto the granulated particles to wrap the enzyme and hold the agglomerate or granule together. This process is economically attractive since the moisture atomized on the carrier is "flashed" as the liquid is atomized on the carrier, and thus a large amount of aqueous enzyme can be loaded onto the carrier.

The three most important parameters for the manufacture of the microgranules (falling within the desired particle size of 20-400μ) are the bed temperature, which should be between about 40-50 ° C and preferably 42-45 ° C, the fluidization air that is 8.5 cubic meters per minute (300 cubic feet per minute-CFM) at the beginning and 17 m3 / min (600 CFM) towards the second half of the process, and a spray rate that in the GPCG granulator size 300 is about 1000 ml up to 1500 ml / minute, and in equivalent granulators such as Uniglatt or Vector FLI it is around 15-20 ml / minute or 20-25 ml / minute, respectively.

A general method useful in the present invention is described below and is further described by the examples that are provided herein. The skilful formulator will recognize variations within the specific parameters of the process, components of the composition, etc., these variations are within the scope of the present invention.

Generally a sugar source such as dissolved corn syrup solids, is dissolved in purified water. This is mixed until the sugar is completely dissolved, after which a modified starch such as Miragel 463 is added to the dissolved sugar solution with mixing, using for example, a high mixer of the propella type. The mixing should continue until the starch is completely hydrated.

This solution can be heated if necessary, to around 40-60 ° C, preferably 45 ° C, until the hydration process is increased. The enzyme, added in a liquid form either directly from the fermentation broth or in concentrated form, is mixed with the binder solution (starch and / or sugar) with mixing. This supplies an appropriate enzyme / binder mixture to be atomized on the carrier.

Meanwhile, the fluid bed granulator, similar to the GPCG 300 made by Glatt Air Techniques, must be preheated to an outlet air temperature of about 60 ° C. The carrier (e.g., soybean meal) is loaded into the preheated mold of the fluid bed granulator and fluidization begins at a low volume of air of about 8.5 m3 / min (300 CFM), sufficient to provide movement in the bed . This is done at a low volume of air because the soy flour is very light and creeps into the filters if a larger volume is used. The atomization rate is then set to about 1 liter to 1.5 liters / minute, and preferably about 1200 ml / minute, and the enzyme / binder mixture is atomized onto the carrier.

In a separate mold, a food grade water soluble polymer (such as Keltone ™ HV) is dispersed and hydrated in purified water at room temperature with mixing. The enzyme / binder mixture is atomized until the mixture is completely finished and then the spray lines must be cleaned with at least 500 ml of purified water. After the lines are washed, the polymer solution is atomized at a rate of 1000 to 1200 ml / minute, a sufficient rate to form a coating and maintain the desired small particle size (20-400μ, preferably 20-200μ) . The excessive volume of atomization must be avoided so that large aggregates are not formed. The polymer solution must be atomized until the solution is finished.

The product is dried with 5-10 minutes of drying time and passed through a mesh or screen of about 45 mesh US (size 350μ) to remove any aggregate of the finished product.

Typical processing conditions useful in the present invention are described in Table I.

Table I. Processing Conditions Uniglatt Vector FLI .Glatt GPCG 300 (or equivalent) Air volume 1.13-1.42 m3 / min 1.13 m3 / min 8.5-9.9 m3 / min at the beginning at the beginning Inlet temperature 45 C (temp, 70-80 C 75-80 C air) (set to maintain 42 SC Exit Air and Temp. 42-45 C 42-45 C 42-45 C Atomization rate 15-20 ml / min 20-25 ml / min 1.2-1.4 lt / min Simple 1.2 mm nozzle 1.2 mm sene. 2.2 mmsenc, Atomization air 0.6-0.85 1.36-1.5 atm 5.44 atm Procedure a. Measure Ion Disintegration Granules Equipment: Mixer of 1000 ml in size and a rotating basket (mesh size of approximately 600 microns) placed on the motor.

Procedure: 1000 ml of deionized water is placed in a blender at room temperature. 500 mg of enzyme granules are weighed in the basket and the basket is closed. The rod of the basket is placed in an engine. The rpm is set to 40 and the basket is lowered into the water beater. The basket is rotated for one minute at 40 rpm and separated from the blender, all the enzyme granules must be disintegrated in the basket.

The preferred solution for the granules described herein is less than or equal to one minute.

The following examples are representative and are not intended to be limiting. Someone skilled in the art can choose other enzymes, cores, particles, methods and coating agents based on these teachings.

Experiments Example 1 448.9 g of ground corn cobs were loaded into a pre-heated Uniglatt fluid bed granulator. 500 ml of liquid cellulase concentrate (5214 μ / ml Multifect CL, commercially available from Genencor International, Inc.) containing 1 g of Miragel 463 (hydrolyzed starch) as a binder, was sprayed onto the ground corn cob at 20 ml / minute, so as not to form aggregates. The bed temperature was maintained between 40-45 C during the spray cycle. 0.1 g of xanthan gum were dispersed and hydrated in 200 ml of deionized water. This solution was atomized on the granulated enzyme / ground corn cob (which were previously ground to a particle size in the range below 100 μ) under conditions similar to those of the previous stage. The product was dried to a moisture level of 5-6%.

Example 2 269.5 g of ground corn cob and 200 g of maltodextrin were loaded into a pre-heated Uniglatt fluid bed granulator. 5 g of Miragel 463 were dispersed and 0. 5 g of Keltone ™ HV in 200 ml of deionized water and hydrated using a homogenizer. This solution was mixed with cellulase liquid concentrate (Multifect CL, commercially available from Genencor International, Inc.) and sprayed on the carrier at 18 ml / minute. The temperature was maintained at 42-45 C during the atomization cycle. The product was dried to a moisture level of 5-6%. The particle size of the starting material was controlled using the starting material in the required range of particle size.

Example 3 446 g of soy semolina were loaded into a pre-heated Uniglatt fluid bed granulator. 25 g of corn syrup solids and 4 g of starch were dispersed (Tender-Jel 479, commercially available from Staleys) were dispersed and hydrated in 200 ml of deionized water. This was mixed with 100 ml of cellulase enzyme (Multifect CL, commercially available from Genencor International, Inc.). The enzyme and binder solution was atomized on the soy semolina. The temperature of the bed during the atomization cycle was maintained at 40-42 C. The product was dried to an exit temperature of 50-52 C.

Example 4 886 g of soy semolina were loaded into a preheated mold of a fluid bed granulator FL-1 (Vector). The binder starch solution was prepared by mixing 10 g of Tender-Jel in 100 ml of deionized water until complete hydration. This solution was mixed in 1000 ml of xylanase concentrate (GC 140, commercially available from Genencor International, Inc.).

A separate coating solution was prepared by dissolving Keltone ™ (commercially available from Kelco) and Maltrin 100 in 200 ml deionized water. The enzyme / binder solution was atomized at 20-25 m / min on the soy semolina, while the fluid bed granulator was maintained at a bed temperature of about 38-40 C. The granulated product was coated using the previously prepared Keltone ™ / Maltrin coating solution. The final product was dried to a bed temperature of 50-52 C.

Example 5 The soy flour was agglomerated using a corn syrup solids base concentrate of 10 g of corn syrup solids per 100 g of soy flour. The corn syrup solids were dissolved in water and atomized at 25 ml / minute on the soybean meal in a fluid bed granulator (Vector FI-1). This agglomerated soybean meal was dried and used as a carrier to make bakery granules using the following procedure: 20 g of Miragel 463 (commercially available from Staleys) (hydrolyzed starch) was dispersed and hydrated in 200 ml of deionized water. This binder solution was mixed with 1500 ml of cellulase (Multifect CL from Genencor International, Inc.). 678 g of soy agglomerate prepared as described above was loaded into a Vector FL-1 fluid bed granulator with an atomization rate of 15 ml / minute. The enzyme / binder solution was atomized on the soy agglomerate. 2 g of Keltone ™ HV (commercially available from Kelco) (algin) were dispersed and hydrated in 660 ml of deionized water. This algin solution was atomized onto the granulated product in the fluidized-milk granulator. The temperature of the bed was maintained at around 40 C during the atomization process. The finished product was dried at a bed temperature of 55 C.

The particle size distribution for the granules manufactured in this example was measured, the data is given in Table II. The data show that most of the particles are between the range of 20-400 micras described here.

Table II Particle Size Distribution for the CSG Multifect Weight Size of the Net Weight *% Mesh Mesh * mesh and the Product Distribution * 425 μ 40.2 40.5 0.3 8.3 250 μ 37.4 40.0 0.6 16.7 150 μ 35.1 36.8 1.7 47.2 106 μ 33.9 34.2 0.3 8.3 90 μ 33.4 33.7 0.3 8.3 75 μ 33.0 33.2 0.2 5.6 63 μ 33.5 33.7 0.2 5.6 Bottom of 217.3 Container * grams Example 6 The product was prepared using the soy agglomerates made using corn syrup solids as the carrier. The binder for the enzyme was 3 gm of Kelgum (commercially available from Kelco) in 200 ml of deionized water. The Kelgum solution was mixed with barley beta-amylase (commercially available from Neson) and atomized at 15-16 ml / minute on the aoya agglomerates in a fluid bed granulator. 2 g of Keltone ™ HV were dispersed and hydrated in 500 ml of deionized water, this algin solution was atomized at 15 ml / minute onto the soybean meal / granulated enzyme at a rate to form a thin coating. The bed temperature of approximately 40 C was maintained during the coating and granulation process. The finished product was dried at a bed temperature of 52-55 C.

Example 7 A batch of cellulase bakery granules were prepared using Miragel 463 starch as the binder. The batch size was 1.0 kg. All procedures were similar to the batch made as per Example 6.

Example 8 A batch of glucose oxidase was made with soy agglomerates using agglomerated soybean meal as the carrier. The granulated product was coated with algin. The batch size was 1.0 kg with 600 ml of liquid enzyme concentrate (OxyGO, commercially available from Genencor International, Inc.) and 0.2% of algin (ie, batch size of 2.0 g per 1.0 kilo).

Example 9 1514.4 g of soybean meal was used as a carrier. 160 g of corn syrup solids were dissolved in 1000 ml of deionized water. 40 g of Miragel 463 (starch) were dispersed and hydrated in the above solution and then mixed with the liquid cellulase. The soybean meal was loaded into the preheated fluid bed granulator (Vector FL-1). The cellulase enzyme / binder solution was atomized at 22-24 ml / minute onto the soybean meal at a rate that did not cause the formation of aggregates. The bed temperature was maintained between 40-45 C during the spray cycle. 4 g of Keltone ™ HV were dispersed and hydrated in 1200 ml of deionized water. This solution was spray coated onto the soybean meal / enzyme granules.

Example 1Q 758 g of soy flour and 20 g of Miragel 463 were loaded into a Vector FL-1 fluid bed granulator. 120 g of corn syrup solids were dissolved with 200 ml of water which was heated to 45 C to aid in the dissolution. The corn syrup solids solution was mixed with 1000 ml of xylanase (GC140, commercially available from Genecor International, Inc.). The mixture of xylanase / corn syrup solids was sprayed onto the soybean meal and the Miragel at an atomization rate of 25 ml / minute. The fluidization rate was adjusted as necessary to accommodate the powder bed when wetted. The bed temperature was maintained between 40/45 C during the spray cycle.

The product was dried for 5 minutes. The final product was dried to a bed temperature of 50-52 C. The product was then separated from the oscillator mold and milled through a US size 50 mesh using an oscillating granulator. 2.0 g Keltone ™ HV was dissolved (Algin) in 400 ml deionized water using a propeller type mixer. The ground product was loaded into the preheated fluid bed granulator Vector FL-1. After cleaning the lines with deionized water, the Keltone ™ HV solution was atomized onto the milled product at a rate of 20 ml / minute. The final product was dried for 5 minutes. The final product was dried to a bed temperature of 50-52 C.

It is noted that with respect to this date, the best method known to the applicant to carry out the invention is that which is clear from the present description of the invention.

Having described the invention as above, the content of the following is claimed as property

Claims (7)

1. A microgranule containing enzymes characterized in that it comprises: a) a suitable carrier b) an aqueous source of enzymes c) one or more binder (s) or disintegrant (s); and d) a food grade polymer coating agent, soluble in water; the microgranule has an average size between 20 and 400 microns.

2. The microgranule according to claim 1, characterized in that the enzyme is selected from one or more of the group consisting of protease, amylase, lipase, cellulase, xylanase, glucose oxidase and mixtures thereof.

3. A method for making a microgranule containing enzymes, characterized in that it comprises: a) loading a suitable carrier into a fluid bed granulator; b) mixing an aqueous source of enzymes and one or more appropriate binders and / or disintegrating agent (s); c) atomizing the enzyme and binder mixture of step b) onto the carrier; and d) atomizing the product of step c) with a food-grade polymer soluble in water at a rate to form a coating and maintaining a particle size from about 20 to 400 microns; with the proviso that steps a) and b) can be carried out in any order.

4. The process according to claim 3, characterized in that it further comprises the preheating of the fluid bed granulator.

5. The process according to claim 3, characterized in that it further comprises starting the fluidization of the carrier in the fluid bed at a low volume of air.

6. The process according to claim 3, characterized in that it further comprises drying the microgranules at a temperature of about 50 C

7. The process according to claim 3, characterized in that it further comprises passing the microgranule through a mesh of a size of about 350 μ.