GRANULAR FEED ADDITIVE

Abstract

The present disclosure relates to a granular feed additive capable of reducing hygroscopicity and lumping and caking, the additive including a basic amino acid and an anion represented by Formula 1, wherein a molar ratio of the anion to the basic amino acid is greater than 0.1 and equal to or less than 0.52.

Claims

1. A granular feed additive comprising a basic amino acid and an anion represented by Formula 1 below, wherein a molar ratio of the anion to the basic amino acid is greater than 0.1 and equal to or less than 0.52:
H.sub.nCO.sub.3.sup.(2-n)−  [Formula 1] (wherein, in Formula 1, n is 0 or 1)

2. The granular feed additive of claim 1, wherein the basic amino acid is one or more selected from the group consisting of lysine, arginine, and histidine.

3. The granular feed additive of claim 1, wherein an average diameter of granules of the granular feed additive is from 0.1 to 3.0 mm.

4. The granular feed additive of claim 1, wherein a pH of the granular feed additive is from 8.5 to 9.5.

5. The granular feed additive of claim 1, wherein a moisture content of the granular feed additive is less than 7 weight % based on a total weight of the granular feed additive.

6. The granular feed additive of claim 1, wherein a content of the basic amino acid is from 50 weight % to 90 weight % based on a total weight of the granular feed additive.

Description

BRIEF DESCRIPTION OF DRAWINGS

[0046] The FIG. 1s a diagram showing steps of preparing a granular feed additive according to an embodiment.

MODE OF DISCLOSURE

[0047] Hereinafter, the present disclosure will be described in more detail with reference to Examples. However, these Examples are for illustrative purposes only, and the scope of the present disclosure is not limited to these Examples.

Examples 1 to 6 and Comparative Examples 1 to 6

[0048] The FIG. 1s a diagram showing steps of preparing a granular feed additive including a high-content basic amino acid according to an embodiment. Hereinafter, each step will be described in detail with reference to the FIGURE.

[0049] 1. Preparation of Mixed Amino Acid Solution

[0050] An amino acid aqueous solution and a concentrated broth were prepared according to compositions shown in Tables 1 and 2, and then, were mixed to prepare a mixed solution. In this Example, L-lysine was used as an example of the basic amino acid. Comparative Examples 1 to 6 were performed in the same manner as in Example 1, except that a L-lysine aqueous solution was used instead of a neutralized L-lysine aqueous solution. First, an amino acid aqueous solution was prepared by purifying a broth containing L-lysine. To prepare the broth, a starter culture of a L-lysine-producing strain of the genus Corynebacterium was performed for 20 hours in 25 mL of a seed medium at pH 7.0 at a speed of 200 rpm at a temperature of 30° C. Here, the seed medium was supplemented with, based on 1 L of distilled water, 20 g of glucose, 10 g of peptone, 5 g of yeast extract, 1.5 g of urea, 4 g of KH.sub.2PO.sub.4, 8 g of K.sub.2HPO.sub.4, 0.5 g of MgSO.sub.4.7H.sub.2O, 100 μg of biotin, 1 mg of thiamine HCl 1, 2 mg of calcium-pantothenic acid, and 2 mg of nicotinamide. A starter obtained by the seed culture was inoculated at 4% (v/v) into a producing medium at pH 7.0 and, while sufficiently ventilating and stirring the medium, the medium was cultured until glucose added thereto was completely consumed, thereby obtaining a final broth. Here, the producing medium was supplemented with, based on 1 L of distilled water, 100 g of glucose, 40 g of (NH.sub.4).sub.2SO.sub.4, 2.5 g of soybean protein, 5 g of corn steep solids, 3 g of urea, 1 g of KH.sub.2PO.sub.4, 0.5 g of MgSO.sub.4.7H.sub.2O, 100 μg of biotin, 1 mg of thiamine HCl, 2 mg of calcium-pantothenic acid, 3 mg of nicotinamide, and 30 g of CaCO.sub.3. After the completion of the culture, a concentration of the L-lysine in the broth was analyzed using HPLC (Waters Company, 2478). A microorganism in the broth was removed by using a membrane having a size of 0.1 μm. The broth from which the microorganism was removed passed through a cation exchange resin tower to absorb L-lysine in the broth and to separate the L-lysine from other impurities. The absorbed L-lysine was desorbed from the resin tower using about 2 N ammonia solution, recovered, and then, heated and concentrated in vacuum, thereby preparing a L-lysine aqueous solution. After the concentration, the L-lysine aqueous solution had a concentration of 560 g/L, a pH of 10.2, a weight of 1.13, and purity of 99 weight %. In the neutralized L-lysine aqueous solution, gas containing 5 volume % of carbon dioxide was injected at a temperature of 50° C. for 10 hours at a rate of 1,000 L/min at 500 rpm after 35 kg of the L-lysine aqueous solution was added to a neutralization tank. The concentrations of the neutralized L-lysine and the bicarbonate ion or carbonate ion following the injection of the carbon dioxide were analyzed using HPLC (Waters Company, 2478). The neutralized L-lysine aqueous solution was the one further containing HCO.sub.3.sup.− or CO.sub.3.sup.2− to the L-lysine aqueous solution. The neutralized L-lysine aqueous solution had a pH of 8.9, a specific gravity of 1.20, and purity of 89 weight %.

[0051] The concentrated broth was prepared by heating and concentrating the broth prepared as described above in a vacuum without performing a purification process. Then, a content of the total solids in the broth after the concentration was set to be 56 weight %.

[0052] The L-lysine aqueous solution or the neutralized L-lysine aqueous solution was mixed with the concentrated broth according to the ratios specified in Tables 1 and 2, thereby preparing a mixed solution. Concentrations of the L-lysine and HCO.sub.3.sup.− or CO.sub.3.sup.2− in the mixed solution were analyzed using HPLC (Waters Company, 2478). Referring to the results of the concentration analysis, results of calculating a molar ratio of HCO.sub.3.sup.− to the L-lysine in the mixed solution in each of Examples 1 to 6 and Comparative Examples 1 to 6 were shown in Tables 1 and 2.

TABLE-US-00001 TABLE 1 Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 Neutral- Neutral- Neutral- Neutral- Neutral- Neutral- ized L- ized L- ized L- ized L- ized L- ized L- lysine Concen- lysine Concen- lysine Concen- lysine Concen- lysine Concen- lysine Concen- aqueous trated aqueous trated aqueous trated aqueous trated aqueous trated aqueous trated solution broth solution broth solution broth solution broth solution broth solution broth Ratio of 100 0 90 10 80 20 70 30 60 40 55 45 lysine in mixed solution (%) Molar 0.62 0.54 0.43 0.32 0.27 0.19 ratio ofHCO.sub.3−/ L-lysine in mixed solution

TABLE-US-00002 TABLE 2 Comparative Comparative Comparative Comparative Comparative Comparative Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 L- L- L- L- L- L- lysine Concen- lysine Concen- lysine Concen- lysine Concen- lysine Concen- lysine Concen- aqueous trated aqueous trated aqueous trated aqueous trated aqueous trated aqueous trated solution broth solution broth solution broth solution broth solution broth solution broth Ratio of 100 0 90 10 80 20 70 30 60 40 55 45 lysine in mixed solution (%) Molar 0.04 0.02 0.02 0.05 0.03 0.02 ratio of HCO.sub.3−/ L-lysine in mixed solution

[0053] As shown in Table 1, as the ratio of the L-lysine aqueous solution increased, the molar ratio of HCO.sub.3.sup.−/L-lysine in the mixed solution decreased. As shown in Table 2, there was no significant change in the molar ratio of HCO.sub.3.sup.−/L-lysine in the mixed solution according to the change in the ratio of the L-lysine aqueous solution.

[0054] 2. Preparation of Granule

[0055] The mixed solution specified in Tables 1 and 2 was then granulated. In detail, the prepared mixed solution was sprayed to be injected into a fluidized bed circulation granulator at a rate of 5 mL/min and at a nozzle pressure of 1.2 kg/cm.sup.2 at a temperature of 80° C. By separation, the prepared granule was selected according to a size from about 0.5 mm to about 3.0 mm.

[0056] 2.1. Analysis of Molar Ratio of HCO.sub.3.sup.− to L-Lysine in Granule and Content of L-Lysine

[0057] To analyze the molar ratio of HCO.sub.3.sup.− to the L-lysine and the content of the L-lysine in the granule of each of Examples 1 to 6 and Comparative Examples 1 to 6, a small content of the granule was dissolved in 1 L of ultrapure water. Then, HPLC (Waters Company, 2478) was performed thereon, and the molar ratio was calculated from the results. Results of the calculation were shown in Tables 3 and 4.

TABLE-US-00003 TABLE 3 Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 Neutral- Neutral- Neutral- Neutral- Neutral- Neutral- ized L- ized L- ized L- ized L- ized L- ized L- lysine Concen- lysine Concen- lysine Concen- lysine Concen- lysine Concen- lysine Concen- aqueous trated aqueous trated aqueous trated aqueous trated aqueous trated aqueous trated solution broth solution broth solution broth solution broth solution broth solution broth Items 100 0 90 10 80 20 70 30 60 40 55 45 pH of 9.2 9.2 9.0 8.9 8.8 8.7 granule (5 weight %) Content 81.6 80.1 80.6 79.5 79.3 79.7 of L- lysine (%) Molar 0.52 0.47 0.36 0.25 0.14 0.10 ratio of HCO.sub.3−/ L-lysine in granule

TABLE-US-00004 TABLE 4 Comparative Comparative Comparative Comparative Comparative Comparative Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 L- L- L- L- L- L- lysine Concen- lysine Concen- lysine Concen- lysine Concen- lysine Concen- lysine Concen- aqueous trated aqueous trated aqueous trated aqueous trated aqueous trated aqueous trated solution broth solution broth solution broth solution broth solution broth solution broth Items 100 0 90 10 80 20 70 30 60 40 55 45 pH of 10.2 10.1 9.8 9.6 9.4 9.3 granule (5 weight %) Content 98.4 94.2 90.2 86.6 83.2 81.7 of L- lysine (%) Molar 0.02 0.03 0.03 0.03 0.02 0.02 ratio of HCO.sub.3−/ L-lysine in granule

[0058] As shown in Tables 3 and 4, it was confirmed that the molar ratio of HCO.sub.3.sup.− to the L-lysine in the granule was in a range of 0.1 to 0.52 in Examples 1 to 6 and in a range of 0.02 to 0.03 in Comparative Examples 1 to 6. In addition, the content of the L-lysine was confirmed to be 78% or more in all of Examples 1 to 6 and Comparative Examples 1 to 6, and accordingly, it was confirmed that the content was high.

[0059] 2.2 Evaluation of Hygroscopicity and Solidification

[0060] To evaluate hygroscopicity and solidification of the granules of Examples 1 to 6 and Comparative Examples 1 to 6, 3 g of each of the granules was placed in a disposable mass plate and stored for one week at a temperature of 40° C. and 60% of relative humidity. Then, changes in moisture in the granule were measured through mass change.

[0061] Additionally, to quantitatively evaluate lumping and caking phenomena (i.e., solidification) of the water-absorbed granules, the granules were placed on a sieve having a mesh size of 1.7 mm, and then, a vibrator was used so that the mass of granules filtered out of the sieve was measured after vibration (50 Hz, 5 minutes) to determine the degree of lumping and caking. The degree of lumping and caking was calculated by the following equation.

[00001]$\mathrm{DEGREE}\mathrm{OF}\mathrm{LUMPING}\mathrm{AND}\mathrm{CAKING}\left(\%\right)=\frac{\begin{array}{c}\mathrm{TOTAL}\mathrm{WEIGHT}\mathrm{OF}\mathrm{GRANULES}-\\ \mathrm{WEIGHT}\mathrm{OF}\mathrm{GRANULES}\mathrm{FILTERED}\mathrm{OUT}\mathrm{OF}\mathrm{SIEVE}\end{array}}{\mathrm{TOTAL}\mathrm{WEIGHT}\mathrm{OF}\mathrm{GRANULES}}\times 100$

[0062] Results are shown in Tables 5 and 6.

TABLE-US-00005 TABLE 5 Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 Neutral- Neutral- Neutral- Neutral- Neutral- Neutral- ized L- ized L- ized L- ized L- ized L- ized L- lysine Concen- lysine Concen- lysine Concen- lysine Concen- lysine Concen- lysine Concen- aqueous trated aqueous trated aqueous trated aqueous trated aqueous trated aqueous trated solution broth solution broth solution broth solution broth solution broth solution broth Items 100 0 90 10 80 20 70 30 60 40 55 45 Moisture 2.7 3.7 4.4 5.4 5.7 6.9 content after 1 week (%) The 1.9 2.1 2.0 3.2 2.9 45.2 degree of lumping and caking after 1 week

TABLE-US-00006 TABLE 6 Comparative Comparative Comparative Comparative Comparative Comparative Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 L- L- L- L- L- L- lysine Concen- lysine Concen- lysine Concen- lysine Concen- lysine Concen- lysine Concen- aqueous trated aqueous trated aqueous trated aqueous trated aqueous trated aqueous trated solution broth solution broth solution broth solution broth solution broth solution broth Items 100 0 90 10 80 20 70 30 60 40 55 45 Moisture 11.2 10.3 10.4 10.1 10.1 10.2 content after 1 week (%) The 99 97 98 96 97 95 degree of lumping and caking after 1 week

[0063] As shown in Tables 5 and 6, the moisture content and the degree of lumping and caking of the granules of Examples 1 to 6 were significantly low compared to those of the granules of Comparative Examples 1 to 6. In particular, in the case of using the L-lysine aqueous solution only (Comparative Example 1), it was confirmed that the highest hygroscopicity was resulted. Also, based on the fact that the hygroscopicity of the granules increased as the proportion of the L-lysine aqueous solution increased in the compositions of Comparative Examples 1 to 6, the polarity of the purified L-lysine was found to increase the hygroscopicity of the granule. Meanwhile, it was also confirmed that, in the granules of Examples 1 to 6, the moisture content and the degree of lumping and caking increased as the proportion of the neutralized L-lysine aqueous solution decreased. That is, as the proportion of HCO.sub.3.sup.− increased in the granule, the polarity of the L-lysine was alleviated, thereby improving the hygroscopicity of the granule. In particular, when the molar ratio of HCO.sub.3.sup.−/L-lysine in the granule decreased to 0.1 or less, the solidification significantly increased. In this regard, it was confirmed that, to solve problems of the solidification, the molar ratio of HCO.sub.3/L-lysine was set to be greater than 0.1.

[0064] Therefore, it was confirmed that, when the molar ratio of HCO.sub.3.sup.− in the granule was greater than 0.1 and equal to or less than 0.52 in the compositions of Examples 1 to 6, the hygroscopicity of the granules may be alleviated, and accordingly that the lumping and caking phenomena caused by the hygroscopicity may be also alleviated.