JP2008109941A - High viscosity locust bean gum and method for producing the same - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide Locust bean gum excellent in viscosity characteristics and dispersibility in water even when the gum is purified one. <P>SOLUTION: A functionally excellent high viscosity Locust bean gum having, when the gum is purified one, 3.5-30 or more times viscosity compared with conventional ones can be prepared by heating, under a specific conditions, a Locust bean gum exhibiting ≤50% loss on drying. <P>COPYRIGHT: (C)2008,JPO&INPIT

Description

  The present invention relates to a high viscosity locust bean gum and a method for producing the same. Such locust bean gum can be used mainly in the food field, but in the cosmetic field, pharmaceutical field or fiber processing field, leather processing field, etc. as an industrial field, thickeners, stabilizers, dispersants, additives, etc. Used as

  Locust bean gum is a polysaccharide extracted from the endosperm of the seeds of carob (Ceratonia siliqua). The structure of locust bean gum is galactomannan mainly composed of β-D-mannose and α-D-galactose. The main chain is 1,4-bonded β-D-mannose, the side chain is bound with 1,6-linked α-D-galactose, and the ratio of D-galactose to D-mannose is approximately D-mannose: D -Galactose = 4: 1. As a method for producing locust bean gum, the skin is removed from the carob fruit, the ground product is extracted with hot water, filtered, precipitated with alcohols such as isopropyl alcohol, the alcohol is removed, dried and ground. Methods are known.

  Locust bean gum is known to produce a highly viscous solution, but so-called unrefined products are yellow and have large powder particles, and if they are simply dissolved in water, they will eventually settle. In order to solve this, many refined products (for example, Saneigen FFI Co., Ltd., trade name “Locust Bean Gum F”) have been put on the market. The actual situation is decreasing. For this reason, the conventional locust bean gum does not sufficiently satisfy the user's needs with respect to the viscosity characteristics. That is, if the locust bean gum has a higher viscosity, the amount added can be further reduced. Accordingly, there has been a demand for locust bean gum having even higher viscosity characteristics in a purified product that is uniformly dispersed. In addition, when a large amount of conventional locust bean gum is put into water, the swollen particles are joined together to form a strong coating around the locust bean gum powder mass, creating a viscous mass called `` Mamako ''. There is a problem that it is not easily dispersed.

  As a result of intensive studies in order to achieve such a problem, the present inventors have found that locust bean gum obtained by heating locust bean gum in a solid state has excellent viscosity characteristics. completed. In the present invention, when an aqueous solution having a locust bean gum concentration of 1.0% by weight is used, it exhibits a viscosity of 2000 mPa · s (B-type viscometer 6 rpm 25 ° C.) or more and is stored at room temperature for 1 week. The present invention relates to a high-viscosity locust bean gum that becomes a homogeneous solution without settling. Similarly, the present invention relates to a high-viscosity locust bean gum having a viscosity of 4000 mPa · s (B-type viscometer 6 rpm 25 ° C.) or more when an aqueous solution having a locust bean gum concentration of 1.0 wt% is used. In any case, the aqueous solution was heated to 80 ° C., stirred with a three-one motor for 1 hour, and allowed to cool to evaluate the viscosity. If the viscosity of 2,000 mPa · s (B-type viscometer 6 rpm, 25 ° C.) or higher is not obtained when an aqueous solution having a locust bean gum concentration of 1.0% by weight is used, the viscosity characteristics are insufficient, and the cosmetics and food fields Even if used as a thickener, stabilizer, dispersant, etc. in the pharmaceutical field, etc., the effect is small and has no value.

  The high-viscosity locust bean gum of the present invention can be obtained by heating locust bean gum having a loss on drying (under normal pressure, heating at 105 ° C. for 5 hours) to 50 wt% or less at 80 to 140 ° C. for 10 seconds to 4 hours. it can. The heating can be performed in gas or liquid. When carried out in a gas, it may be colored if carried out in the presence of oxygen, such as in the air, so it is better to carry out in an inert gas. Coloring can also be avoided by heating in gas under reduced pressure. When heating in a liquid, it is heated in a state where the locust bean gum is dispersed in an inert solvent that does not dissolve the locust bean gum. Coloring does not occur when heating in liquid.

  The high-viscosity locust bean gum of the present invention is an extremely excellent water-soluble thickener having viscosity characteristics several times that of conventional locust bean gum, even if the raw locust bean gum is refined. With a small amount of addition, an effect higher than that of the conventional product can be obtained, water dispersibility is improved, and workability is good.

  The present invention is described in detail below. As described above, the high viscosity locust bean gum of the present invention generally has a weight loss on drying (under normal pressure, 105 ° C., 5 hours heating, unless otherwise defined below) “weight loss on drying” refers to weight loss on drying under these conditions. Can be obtained by heating locust bean gum of 50% by weight or less at 80 to 140 ° C. for 10 seconds to 4 hours. The raw locust bean gum used to produce the highly viscous locust bean gum of the present invention is a locust bean gum having a loss on drying of 50% by weight or less, preferably 20% by weight or less, more preferably 15% by weight or less. In addition, when the raw product is used as a raw material, the same viscosity characteristics can be obtained. However, the present invention does not have the function of suppressing sedimentation of the locust bean gum. It is essential to use it. As such raw material locust bean gum, commercially available locust bean gum in the form of powder or granules can be used. If the loss on drying of the raw locust bean gum is more than 50% by weight, the product temperature of the locust bean gum is not sufficiently increased, and there is no effect of improving the viscosity. In order to produce the highly viscous locust bean gum of the present invention, the raw locust bean gum is heated. The heating is 80 to 140 ° C., preferably 100 to 130 ° C., more preferably 105 to 125 ° C., and more than 10 seconds. , Preferably 10 seconds to 4 hours, more preferably 10 seconds to 3 hours. Even under these conditions, heating for a relatively short time on the high temperature side and heating for a relatively long time on the low temperature side are preferable. When the heating temperature is less than 80 ° C., the viscosity is not sufficiently improved, and when it exceeds 140 ° C., the possibility of coloring generally increases.

  The heating can be performed in gas or liquid. When carried out in a gas, it may be colored if carried out in the presence of oxygen, such as in the air, so it is preferable to carry out in an inert gas that does not react with locust bean gum. Examples of the inert gas include nitrogen gas, helium gas, carbon dioxide gas, and water vapor. Coloring can also be avoided by heating in gas under reduced pressure. Of course, the inert gas can be used as the gas in this case, but air can also be used without coloring depending on the degree of decompression. The degree of decompression is not particularly limited, but 200 to 0.01 mmHg is appropriate.

  When heating in a liquid, it is heated in a state where the locust bean gum is dispersed in an inert solvent that does not dissolve the locust bean gum. Coloring does not occur when heating in liquid. The inert solvent is not particularly limited as long as it does not dissolve locust bean gum and does not react with locust bean gum. Examples of inert solvents include methanol, ethanol, n-propanol, isopropanol, n-butanol, n-pentyl alcohol, n-hexyl alcohol, etc., alkanols having 1 to 6 carbon atoms, 1,3-butylene glycol, propylene glycol Mono- or di-lower of ethylene glycol such as ethylene glycol and other alkanediols having 1 to 4 carbon atoms, ethylene glycol dimethyl ether, ethylene glycol diethyl ether, ethylene glycol monomethyl ether (methyl cellosolve), ethylene glycol monoethyl ether (ethyl cellosolve), etc. Alkyl (C = 1-4, especially 1-2) ether, diethylene glycol, diethylene glycol dimethyl ether, diethylene glycol diethyl ether, diethylene glycol Monomethyl ether, diethylene glycol monoethyl ether, diethylene glycol mono- or di-lower alkyl (C = 1 to 4, in particular 1 to 2) and diethylene glycol monobutyl ether and ether and the like. The reaction in an inert solvent can optionally be carried out under pressure, for example in an autoclave.

  Isolation of the high-viscosity locust bean gum obtained after the heat treatment can be performed, for example, by filtering the heat treatment liquid, washing the cake with a low-boiling solvent such as ethanol, if necessary, and then vacuum drying. The high viscosity locust bean gum of the present invention produced by the above method is different from the conventional locust bean gum in its high viscosity. That is, the high-viscosity locust bean gum of the present invention is 2000 mPa · s (mPa · s = millipascal × second) (B-type viscometer, 6 rpm, 25 when the locust bean gum concentration is 1.0% by weight aqueous solution. Unless otherwise defined below, the viscosity value refers to that under this condition, where 1 mPa · s = 1 cP (centipoise) or more. Since the viscosity of a 1.0% by weight aqueous solution of commercially available locust bean gum (refined product) is about 80 to 1200 mPa · s, the high viscosity of the locust bean gum of the present invention is amazing.

  Regarding other physical properties of the highly viscous locust bean gum of the present invention, it is considered that there is no change in molecular formula as compared with the conventional locust bean gum except that the molecular weight is poor in reproducibility under measurement conditions. For example, the NMR spectrum, elemental analysis, and IR spectrum (KBr method and FT-IR method) are substantially unchanged compared to the raw locust bean gum. The high-viscosity locust bean gum of the present invention can be used in the same applications as conventional locust bean gum, but at that time, it can exhibit a thickening effect more than expected with a smaller dose than the conventional product. Moreover, water dispersibility is also improved and workability is good. Such highly viscous locust bean gum of the present invention can be used alone or in combination with other water-soluble gelling agents and emulsifiers to obtain stable gels and emulsions. Therefore, the high-viscosity locust bean gum of the present invention can be used as a water-soluble thickener in fields such as food, cosmetics, pharmaceuticals, and general industrial fields including the petroleum industry. Furthermore, the locust bean gum of the present invention exhibits a higher viscosity value on the low temperature side. For this reason, the function can be exhibited even in applications such as frozen foods, frozen desserts, and ice desserts. The present invention will be specifically described below with reference to Examples, Comparative Examples, and Reference Examples, which are intended to illustrate the present invention and do not limit the present invention in any way.

Comparative Example 1
As a commercially available locust bean gum, the locust bean gum (trade name: “Locust bean gum F” 3% by weight loss on drying) obtained from San-Ei Gen FFI Co., Ltd.) was weighed to give a 1.0% by weight aqueous solution, The mixture was stirred with a three-one motor for 1 hour while being heated to 80 ° C., allowed to cool, and then the viscosity was measured the next day (Sample No. 1). The viscosity was measured using a B-type viscometer (manufactured by Tokyo Keiki Co., Ltd.) under the condition of 6 rpm.

  Comparative example 2 and 3 Locust bean gum (trade name: “Bistop D-6”, 8% by weight loss on drying) obtained from San-Ei Gen FFI Co., Ltd. was used as a commercially available locust bean gum. The solution was prepared and the viscosity was evaluated (Sample No. 2). In addition, the same solution adjustment and viscosity evaluation were performed using locust bean gum (trade name: “Locust Coal” 5% by weight loss on drying) obtained from Sanei Pharmaceutical Trading Co., Ltd. as a crude product (Sample No. 3). ). These results are shown together in Table 1.

Example 1
10 g of locust bean gum powder (obtained from San-Ei Gen FFI Co., Ltd., trade name “Locust bean gum F”, loss on drying 3% by weight) was dispersed in 40 g of 1,3-butylene glycol and heated at 120 ° C. for 20 seconds. . Each locust bean gum dispersion was filtered and the cake was washed with 40 g of ethanol. Vacuum drying was performed for 12 hours to remove ethanol to obtain a highly viscous locust bean gum (Sample No. 4). Each 1.0 weight% aqueous solution was prepared similarly to the comparative example 1, and the viscosity was measured. A significant increase in viscosity was observed. As compared with the locust bean gum of Comparative Example 1, the dispersion of each locust bean gum in water was less likely to cause “mamako” and improved dispersibility.

Example 2
Locust bean gum powder (obtained from San-Ei Gen FFI Co., Ltd., trade name “Bistop D-6”, loss on drying 8% by weight) is dispersed in 40 g of 1,3-butylene glycol and heated at 90 ° C. for 2 hours. did. Each locust bean gum dispersion was filtered and the cake was washed with 40 g of ethanol. Vacuum drying was performed for 12 hours to remove ethanol and obtain a highly viscous locust bean gum (Sample No. 5). Each 1.0 wt% aqueous solution was prepared and the viscosity was measured. A significant increase in viscosity was observed. As compared with the locust bean gum of Comparative Example 2, the dispersion of each locust bean gum in water was less likely to cause “mamako” and improved dispersibility.

Example 3
10 g of locust bean gum powder (obtained from San-Ei Gen FFI Co., Ltd., trade name “Bistop D-6”, loss on drying 8 wt%) was heated at 115 ° C. for 3 hours under reduced pressure (air, 60 mmHg) (sample No. 6). A 1.0% by weight aqueous solution of the resulting high viscosity locust bean gum was made and the viscosity was measured. A significant increase in viscosity was observed. As compared with the locust bean gum of Comparative Example 2, the dispersion of each locust bean gum in water was less likely to cause “mamako” and improved dispersibility.

Example 4
Locust bean gum powder (obtained from San-Ei Gen FFI Co., Ltd., trade name “Bistop D-6”, loss on drying 8% by weight) 10 g of water to reduce the loss on drying to 45% by weight, then in nitrogen The sample was heated at 115 ° C. for 3 hours (Sample No. 7). A 1.0% by weight aqueous solution of the resulting high viscosity locust bean gum was made and the viscosity was measured. A significant increase in viscosity was observed. As compared with the locust bean gum of Comparative Example 2, the dispersion of each locust bean gum in water was less likely to cause “mamako” and improved dispersibility.

Example 5
10 g of locust bean gum powder (obtained from Sanei Pharmaceutical Trading Co., Ltd., trade name “Locust Coal”, loss on drying 5% by weight) was heated in soybean oil at 110 ° C. for 1 hour (sample No. 8). The resultant was washed with hexane and dried to prepare a 1.0% by weight aqueous solution of the resulting highly viscous locust bean gum, and the viscosity was measured. A significant increase in viscosity was observed. Dispersion of each locust bean gum in water was less likely to cause “mamako” and improved dispersibility compared to locust bean gum of Comparative Example 3 (Sample No. 3). The results of these examples are shown in Table 2.

It is a general formula of locust bean gum. Statistically, one galactose is bound to four mannoses.

Claims (2)

When an aqueous solution having a locust bean gum concentration of 1.0% by weight is used, it exhibits a viscosity of 2000 mPa · s (B-type viscometer 6 rpm, 25 ° C.) or higher and does not settle when the aqueous solution is stored at room temperature for 1 week. High viscosity locust bean gum that becomes a homogeneous solution. A high-viscosity locust bean gum having a viscosity of 4000 mPa · s (B-type viscometer 6 rpm 25 ° C.) or more when an aqueous solution having a locust bean gum concentration of 1.0% by weight is used.

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