JP2006206713A - Sterilized pectin and method for producing the same - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To obtain sterilized pectin by killing pectin-derived Alicyclobacillus to the extent in which function of pectin is not spoiled and provide an efficient method for producing the same and a preferable application of the same. <P>SOLUTION: The method for producing pectin is to wet grind pectin dispersed in an organic solvent by bead mill and kill bacteria of the genus Alicyclobacillus in pectin. It is preferable to grind pectin to have 0.1-1 μm average size. Sterilized pectin is preferably used for producing acidic beverages. <P>COPYRIGHT: (C)2006,JPO&NCIPI

Description

  The present invention relates to a sterilized pectin and a method for producing the same. Specifically, the present invention relates to a sterilized pectin obtained by sterilizing Alicyclobacillus bacteria present in pectin, a method for producing the pectin, and a method for producing an acidic beverage using the sterilized pectin.

  Pectin is a water-soluble vegetable fiber widely used in the fields of food, cosmetics, pharmaceuticals and the like. Pectin is usually distributed as a powder product having a size of 100 μm to several mm. Moreover, it insolubilizes and precipitates in organic solvents, such as ethanol and isopropanol. Utilizing this phenomenon, a method is known in which pectin is wet-pulverized in an organic solvent by a bead mill to reduce the molecular weight.

In the food field, pectin is mainly used for the production of jam, marmalade, fruit preparation, jelly, pudding, dessert base, noodles, bread, various beverages and the like as a stabilizer, gelling material or thickening material. For example, in an acidic milk beverage, pectin has been conventionally added as a stabilizing material in order to prevent casein protein derived from milk from aggregating and precipitating to impair the appearance and texture. Recently, however, the presence of alicyclobacillus bacteria in pectin has become a problem for acidic beverages.

  An alicyclobacillus bacterium is an aerobic spore-forming bacterium that has been detected in recent years due to a deterioration accident involving the odor of acidic beverages, and has a characteristic ω-cyclohexane fatty acid as a main cell fatty acid. The general shape of Alicyclobacillus bacteria is a gonococcus having a width of 0.7 to 1 μm and a length of 3 to 5 μm, and forms spores at the end of vegetative cells. A colony is formed on a YSG agar medium and can grow in a temperature range of 20 to 70 ° C. and a pH range of 2 to 6 (Non-patent Document 1).

  Thus, the Alicyclobacillus bacterium is a heat-resistant acidophilic bacterium and has high heat resistance and acid resistance. Therefore, heat treatment in a normal beverage production line (that is, 120 ° C. · 4 at pH 4.6 or higher). It is characterized in that it does not die if it is 85 ° C./30 minutes at pH 4 or higher, and sterilized by the Ministry of Health and Welfare Notification such as 65 ° C./10 minutes at pH 4.0 or lower. Although Alicyclobacillus bacteria are not pathogenic, they may cause a phenol-like off-flavor and impair the commercial value of the food. It is known that about 300 / g alicyclobacillus bacteria are usually present in unsterilized pectin.

  Alicyclobacillus bacteria are killed by heating pectin or food and drink to which this is added at an extremely high temperature, but such treatment is damaged by pectin itself and functions as a food additive (stabilization). Performance, gelation ability, thickening function, etc.). Moreover, the heating at high temperature deteriorates the flavor of food and drink, causes loss of nutritional components, and impairs the commercial value.

  In addition, about the fruit juice in which an alicyclobacillus genus bacteria exists like pectin, the method of carrying out the membrane filtration of the fruit juice or fruit juice drink directly can be taken. However, in the case of pectin, when this is added, the solution becomes extremely viscous, so that the membrane filtration method has poor working efficiency and cannot be employed.

WO01 / 095747 Japanese Patent Laid-Open No. 5-15317 JP 2003-160411 A JP 2004-187585 A Published December 10, 2004 by Kenshisha Co., Ltd. “Thermophilic acidophilic bacteria-Alicyclobacillus genus bacteria” (edited by the Microbiology Subcommittee of ILSI Japan Food Safety Research Group)

Patent Document 1 discloses a water extract of grape seeds and / or grape fruits in an acidic beverage in order to suppress the growth of thermostable eosinophils belonging to the genus Alicyclobacillus in the acidic beverage. A method of blending a water extract of squeezed rice cake is disclosed. However, this method is a method for suppressing the growth of heat-resistant acidophilic bacteria, and is not a method for sterilizing or removing heat-resistant acidophilic bacteria.

  In Patent Document 2, a hydrogel of dietary fiber containing pectin is forcibly pushed into a grinding medium such as a bead mill built in a container and wet-pulverized to produce a large amount of fine particle hydrogel having an average particle size of 20 μm or less. A method of obtaining is disclosed. However, Patent Document 2 does not disclose any application of this method to a method for sterilizing or removing Alicyclobacillus bacteria in pectin.

  In addition, for foods and drinks containing heat-resistant acidophilic bacteria such as Alicyclobacillus bacteria, Patent Literature 3 is added with a fungus inhibitor containing diglycerin myristic acid ester and / or a salt thereof as an active ingredient. A method for inhibiting the growth is disclosed. Furthermore, Patent Document 4 discloses a method of suppressing the action of heat-resistant acidophilic bacteria by adding a quality deterioration preventing agent containing polyglycerin fatty acid ester or lecithin. However, the addition of these fungicide inhibitors and quality deterioration inhibitors affects the flavor of food and drink, and in recent years, there is a tendency to be avoided by consumers with increased safety preferences. When a fall prevention agent is added, there is a high risk of receiving an image down as a food or drink. Moreover, these bacteria inhibitors and quality deterioration inhibitors only suppress the activity of heat-resistant acidophilic bacteria, and do not sterilize or remove heat-resistant acidophilic bacteria.

  Non-Patent Document 1 describes general properties and physiological / biochemical properties of Alicyclobacillus bacteria. However, Non-Patent Document 1 does not disclose anything about sterilization and removal by pulverizing a sample containing bacteria belonging to the genus Alicyclobacillus.

  As described above, none of the known literatures disclose a method for sterilizing Alicyclobacillus bacteria. Therefore, a method for sterilizing or removing alicyclobacillus bacteria in pectin without damaging the function of pectin and without losing the flavor of foods and drinks to which pectin is added has not been developed yet. Conceivable.

  In view of the above situation, an object of the present invention is to provide a pectin obtained by sterilizing a pectin-derived alicyclobacillus genus bacterium without impairing its function as a pectin, a method for producing the same, and a use thereof.

  Among the present inventions for solving the above-mentioned problems, the invention described in claims 1 and 2 is directed to wet pulverization of pectin dispersed in an organic solvent using a bead mill, and alicyclobacillus bacteria present in pectin. Is a method of producing pectin sterilized.

  The invention described in claim 2 is a method for producing pectin sterilized from Alicyclobacillus bacteria according to claim 1, wherein pectin is pulverized to an average particle size of 0.1 μm to 1 μm. is there.

  The invention described in claim 3 is a pectin obtained by sterilizing Alicyclobacillus bacteria sterilized by the method according to claim 1 or 2.

  The invention described in claim 4 is a method for producing an acidic beverage using the sterilized pectin according to claim 3.

  According to the present invention, it is possible to provide a pectin that has been sterilized from the genus Cyclobacillus genus derived from pectin, an efficient production method thereof, and a suitable application without impairing the function as a pectin. Can be greatly expanded. Further, according to the present invention, it is possible to easily produce an acidic beverage that is free from the risk of contamination with Alicyclobacillus bacteria. Thus, this invention can provide industrially useful pectin, its efficient manufacturing method, and its suitable use, without impairing the value and image of food and drink to be added.

  The method for producing sterilized pectin according to the present invention is a method in which pectin and beads are coexisted in an organic solvent, and pectin and beads are collided using centrifugal force, stirring force, etc., and pectin is finely divided. It is. Specifically, utilizing the property that pectin is insolubilized and precipitated in an organic solvent solution, a dispersion liquid in which pectin is dispersed in an organic solvent is circulated through a bead mill, and the pectin and beads are collided between the pectin and the beads. This is a method of pulverizing and sterilizing Alicyclobacillus genus bacteria present in pectin by crushing between them and performing wet pulverization. As a method for crushing pectin, in addition to a method using a bead mill as in the present invention, a method using a jet mill (a method of crushing powder by colliding with a pressure-injected gas: test example 2 described later) A method of dry pulverization such as the method of Comparative Example 2) or a method of drying an aqueous solution of pectin after ultra-high temperature treatment (for example, heating at 120 ° C. for 30 minutes), adding several times the amount of alcohol to precipitate pectin, (Method of Comparative Example 3), but as shown in Test Example 2, the dry pulverization method does not have sufficient sterilizing effect of pectin, and the pectin is damaged by the ultra-high temperature treatment method. Cannot be adopted.

  In addition, a low-concentration pectin solution (about 0.1 to 0.3%) having a relatively low viscosity is passed through a membrane having a filter diameter of 0.1 μm or less to remove Alicyclobacillus bacteria remaining as a residue on the filtration membrane. Although the method (the method of Comparative Example 4 in Test Example 2 described later) is also conceivable, such a filtration membrane method has a slow filtration rate, and after that, the filtrate is concentrated to obtain several times the amount of alcohol. In addition, this method cannot be adopted because of the great labor and time constraints such as pectin must be precipitated, dried and ground.

  For the reasons described above, the present invention employs the bead mill method that has been used to reduce the molecular weight of pectin. In the present invention, any type of beads may be used, but those having a particle size of about 0.01 to 1 mm are preferably used. The beads need not be edible because they can be completely removed with a filter after sterilizing the pectin, but they are less toxic if used for edible purposes, and may be broken by collision during crushing. Those having no strength are desirable. Examples thereof include nylon, ceramic and zirconia. In the present invention, any type of bead mill can be used.

  The organic solvent used in the present invention may be of any type as long as it does not dissolve pectin, but it can be evaporated with a spray dryer after pulverization, and the residual amount should be safe. Those that can be used are preferred, and examples thereof include ethanol and isopropyl alcohol.

  Any pectin may be used in the present invention. For example, high methoxyl pectin, low methoxyl pectin, and amide pectin are used as chemical compositions, and thickening pectin, stabilizing pectin, and gelling pectin are used as applications. As the state, powders, slurries, and plants as raw materials can be exemplified by fruits and vegetables.

  In the present invention, the pectin concentration (dispersion degree) in the organic solvent and the bead concentration (dispersion degree) may be combined in any combination. However, if the concentration of both is too high, the fluidity of the solvent decreases. Work efficiency falls. On the other hand, if it is too low, the frequency of collisions will decrease and work efficiency will decrease. Usually, by adjusting the bead concentration to a solution ratio of several percent to 50% and the pectin concentration to a solution ratio of several percent to 50%, a sufficiently high collision frequency and fluidity can be obtained. Can do.

  In the present invention, when wet-pulverizing pectin in an organic solvent using a bead mill, the temperature of the bead mill tends to increase due to friction during crushing due to repeated collisions between the beads and pectin. Since cooling can be sufficiently performed, there is no possibility that pectin is damaged by heat and its function is impaired. Further, in the wet pulverization according to the present invention, only organic solvent and beads are used, and both can be removed after pulverization, so that it is safe and does not cause anxiety to consumers. Sterilization can be performed.

  The method of removing the beads and the organic solvent from the pectin dispersion after sterilization is as follows. That is, for the beads, the difference in particle size between the beads and pectin is utilized to separate them using a rotor centrifugal force and a filter. Pectin is pulverized to a size smaller than that of beads, and can be easily separated with a sieve or a filter. The obtained mixture of sterilized pectin and organic solvent is removed by evaporating the organic solvent by drying.

  In the present invention, since the size of Alicyclobacillus bacteria is about 0.5 to 5 μm, pectin has a mean particle size of 0.1 μm to 1 μm to sterilize Alicyclobacillus bacteria. It is preferable to pulverize.

The sterilized pectin produced in this way can be used as a stabilizing material, a gelling material, and a thickening material for the production of various foods and beverages, as in the past, but especially for acidic milk beverages and acidic fruit juice beverages. It is preferably used for the production of acidic beverages.
A general method for producing an acidic beverage using pectin is as follows.
First, pectin is dispersed in water, heated to about 90 ° C. and dissolved, and if it is an acidic milk beverage, milk is added and mixed by stirring. To this, an acidic raw material such as fruit juice or citric acid is added, and the pH is adjusted from 3.7 to 4.0. In the case of an acidic fruit juice drink, no milk ingredients are added. While maintaining the raw material solution thus adjusted at about 60 ° C., it is homogenized at a high pressure of about 150 kg / cm 2. Sterilize at 90 ° C. for 15 seconds and aseptically fill the container. Acidic beverages can be produced using pectin that has been sterilized with Alicyclobacillus bacteria in the same manner as described above.

Hereinafter, the present invention will be described in more detail with reference to examples and test examples. In the present invention, “%” indicates a weight percentage unless otherwise specified.
In the present invention, the number of living Alicyclobacillus bacteria is determined based on the “Japan Fruit Juice Association Method” (a method of selectively detecting cultivated Alicyclobacillus bacteria near the optimum growth temperature). The number of viable bacteria in 1 mL (or 1 g) is measured.

<Production Example 1 of Sterilized Pectin>
The pectin was dispersed while stirring a 30% pectin (degussa. Texturant Systems: UNIPECTIN AYD30) / isopropyl alcohol solution in a tank. This dispersion was sent from a tank to a bead mill and circulated for 5 hours, and wet pulverization was repeated by repeatedly causing the pectin to collide with the beads. The beads were made of nylon with a particle size of 0.3 mm, and the dispersion was circulated while rotating at 2000 rpm. The tank and the bead mill were equipped with a cooler, and cooled by circulating water at 4 to 5 ° C. The pulverized pectin dispersion was separated and collected through a filter by the centrifugal force of the bead mill rotor and applied to a spray dryer to obtain granular sterilized pectin. The number of living Alicyclobacillus bacteria in the obtained sterilized pectin was 38 / g. Moreover, as a result of measuring with a laser particle meter, the average particle diameter of the obtained sterilized pectin was 1 μm.

<Production Example 2 of Sterilized Pectin>
The pectin was dispersed while stirring a 30% pectin (degussa. Texturant Systems: UNIPECTIN AYD30) / isopropyl alcohol solution in a tank. This dispersion was sent from a tank to a bead mill and circulated for 5 hours, and wet pulverization was repeated by repeatedly causing the pectin to collide with the beads. The beads were made of a ceramic material having a particle diameter of 0.1 mm, and the dispersion was circulated while rotating at 3000 rpm. In order to increase the pulverization efficiency, 100% ethanol was allowed to flow through the tank and bead mill cooler as a solvent, and the temperature of the liquid in the tank was maintained at -20 ° C to -30 ° C during the pulverization. The pulverized pectin dispersion was separated and collected through a filter by the centrifugal force of the bead mill rotor and applied to a spray dryer to obtain granular sterilized pectin. The number of viable bacteria of the genus Alicyclobacillus in the obtained sterilized pectin was 0 / g. Moreover, as a result of measuring with a laser particle meter, the average particle diameter of the obtained sterilized pectin was 0.6 μm.

<Example of production of acidic milk drink using sterilized pectin>
The sterilized pectin prepared in Example 2 was added to 70 ° C. warm water, and 500 kg of 1% pectin solution was obtained while stirring with a high-speed stirrer. Separately, skim milk powder was dissolved in warm water of about 40 ° C. to obtain 400 kg of 3% skim milk powder solution. After mixing 300 kg of 1% pectin solution, 96 kg of sugar and 367 kg of 3% nonfat dry milk solution, 1 kg of citric acid was further added and stirred, and 236 kg of water was added to make the solution 1000 kg. This solution was subjected to a homogenization treatment at 150 kg / cm 2 by applying a high-pressure homogenizer. This was sterilized by heating at a temperature of 90 ° C. with a plate heat exchanger, aseptically filled into a container and cooled to obtain a creamy acidic milk beverage free from off-flavors. The number of living Alicyclobacillus bacteria in the obtained acidic milk beverage was 0 / mL. Moreover, although the obtained acidic milk drink filled with the container was stored in a room at 5 ° C. for 30 days, none of the creamy properties changed.

Test example 1

<Pectin grinding test using bead mill>
(1) Test method HM pectin ("UNIPECTIN AYD30" manufactured by degussa.Texturant Systems) was crushed (sample 1 and sample 2) or without pulverization (sample 3). Then, after culturing by adding to a YSG agar medium (culture conditions pH 3.7 · 45 ° C.), the number of living Alicyclobacillus bacteria in the sample was measured.
(1) Test sample:
I. Sample 1: Fine powder (average particle size: about 0.9 μm)
Commercially available waxy methoxyl pectin was mixed with 100% ethanol to make a 30% dispersion. This pectin dispersion is circulated for 1 hour while rotating at 2000 rpm on a bead mill containing ceramic beads (particle size: 0.2 mm). The pectin is crushed by colliding the pectin with the beads and collected from the bead mill. I made one.
B. Sample 2: Coarse powder (average particle size of about 12 μm)
Specimen 2 was prepared by pulverizing the same kind of commercially available pectin by the same method as Specimen 1 except that another ceramic bead (particle size 1 mm) was used.
C. Sample 3: Unground (average particle size of about 100 μm)
Commercially available pectin was used as it was without crushing.
(2) Preparation of YSG agar medium:
I. Composition: Liquid A Yeast extract (Difco) 0.4%, glucose 0.2%
B liquid soluble starch (Difco) 0.4%, agar 0.3%
B. Preparation:
Solution A was adjusted to pH 3.7, and both solutions A and B were autoclaved (121 ° C., 20 minutes). Thereafter, both A and B solutions were mixed to obtain a YSG agar medium.
(3) Sample preparation method:
I. 20-fold diluted sample: 5 g of each specimen was dissolved in 95 mL of physiological saline (diluted 20-fold) and incubated (heat shock) for 20 minutes in a water bath at 70 ° C.
B. 100-fold diluted sample: 2 mL of 20-fold diluted sample was placed in a test tube and diluted with 8 mL of water. C. 1 mL of each sample was collected in a petri dish, and YSG agar medium was dispensed and mixed.
D. Thereafter, 5 plates were cultured per specimen (45 ° C., 5 days). This corresponds to the number of living Alicyclobacillus in 0.25 g and 0.05 g of pectin, respectively.

(2) Test results The test results are as shown in Tables 1 and 2.
<Table 1>
Viable count (total of 5 plates)
20-fold diluted sample 100-fold diluted sample Specimen 1 (fine powder) 7 2 Specimen 2 (coarse powder) 78 19 Specimen 3 (unground) 249 120 120 << Table 2 >>
Number of viable bacteria per gram of pectin (calculated from 20-fold diluted sample)
Specimen 1 (fine powder) 28 Specimen 2 (coarse powder) 312 Specimen 3 (unground) 996

(3) Discussion From Tables 1 and 2, it was confirmed that the number of Alicyclobacillus bacteria decreased as pectin was finely ground.
Alicyclobacillus bacteria have durable organs called spores, which are resistant to heat and acid, but the cells are destroyed together with the spores by physically finely grinding them with a bead mill. It is thought that the number of viable bacteria decreases.

Test example 2

（注１）ペクチンの平均粒子径は、試作５回の平均値であり、レーザー
粒子計により測定した。
（注２）ペクチンの処理効率は、表３に示す処理を行なうについて１時間に処理することが可能な量を測定したものである。 <Production test of acidic beverage>
(1) Test method Pectin (5 types) with properties shown in Table 3 each 0.3%, milk 11.6%, granulated sugar 9.6%, citric acid 0.1%, fresh water 78.4% (total 100) %), An acidic milk drink was made as a prototype.
(2) Manufacturing method of test pectin All five types of pectin used for the test are commercially available products of the same type, and are all powdery.
In Comparative Example 1, commercially available pectin (high methoxyl pectin AYD30 from Degussa.Texturant Systems) was used as it was.
In Comparative Example 2, pectin (average particle size of 10 μm) that was dry-ground using a jet mill was used.
In Comparative Example 3, pectin was hydrated in water, treated at high temperature and high pressure (120 ° C. for 30 minutes), then added with about 4 times the amount of alcohol to precipitate pectin, dried, and pulverized. .
In Comparative Example 4, a low-concentration pectin solution (about 0.1 to 0.3%) having a relatively low viscosity was passed through a membrane having a filter diameter of 0.1 μm or less, and the Alicyclobacillus bacteria remaining as a residue on the filtration membrane The filtrate was added with 4 times the amount of ethanol to precipitate pectin, and dried and powdered pectin was used.
In the example of the present invention, pectin sterilized by the same method as in Example 1 was used.

(Note 1) The average particle diameter of pectin is an average value of five trial productions, and was measured with a laser particle meter.
(Note 2) The processing efficiency of pectin is a measure of the amount that can be processed per hour for the processing shown in Table 3.

(3) Prototype results Table 4 shows the results of trial production of acidic milk beverages.

From Table 4, regarding Comparative Example 1, the beverage was stabilized, but the presence of Alicyclobacillus bacteria was confirmed.
Regarding Comparative Example 2, it was confirmed that the beverage was stabilized but the bactericidal effect was insufficient.
As for Comparative Example 3, it was confirmed that although sufficient sterilization was performed, the pectin was damaged and the stabilizing ability was impaired.
Regarding Comparative Example 4, the beverage was stabilized and a bactericidal effect was also observed, but it was confirmed that the processing efficiency of pectin was extremely poor.
Regarding the inventive examples, it was confirmed that the beverage was stabilized, the bactericidal effect was sufficient, and the processing efficiency of pectin was very high.

(4) Discussion From the above results, it was found that the method of dispersing pectin in an organic solvent and wet-grinding using a bead mill is the most effective for killing Alicyclobacillus bacteria. That is, it was confirmed that the method of the present invention has the highest bactericidal effect and is efficient.

Industrial availability

  According to the present invention, since the Alicyclobacillus bacteria derived from pectin can be efficiently sterilized without impairing the function as pectin, the present invention can greatly expand the use of pectin. Further, according to the present invention, it is possible to easily produce an acidic beverage that is free from the risk of contamination with Alicyclobacillus bacteria. Therefore, the present invention can provide a very useful pectin, its efficient production method, and its preferred use.

Claims (4)

  A method of producing pectin in which pectin dispersed in an organic solvent is wet-ground using a bead mill to sterilize Alicyclobacillus bacteria existing in pectin.   The method for producing pectin obtained by sterilizing Alicyclobacillus bacteria according to claim 1, wherein the pectin is pulverized to an average particle size of 0.1 µm to 1 µm.   A pectin having sterilized Alicyclobacillus genus bacteria sterilized by the method according to claim 1 or 2. A method for producing an acidic beverage using the sterilized pectin according to claim 3.