JPS62126951A - Production of sweetener containing glucide source for proliferation of bifidus bacteria - Google Patents

Abstract

PURPOSE:To obtain a high-quality sweetener having bifidus-proliferation effect, in high efficiency, eliminating the C-crystallization step of the conventional sugar-refining process and improving the recovery of raffinose, by repeating the crystallization of desalted beet sugar syrup and subjecting the separated crude syrup for crystallization to chromatographic separation. CONSTITUTION:Beet syrup desalted with ion exchange resin is repeatedly crystallized and the separated crude syrup for crystallization is subjected to chromatographic separation. The syrup is separated into a fraction containing supersaturated raffinose at normal temperature, a fraction containing high-purity sucrose and a fraction rich in betaine. The fraction containing high-purity sucrose is recycled to a recovery process and the raffinose fraction is concentrated optionally after converting to an oligosaccharide with a transferase. In the case of mixing a raffinose-containing sugar with powdery sugar, it is preferable to add a reduced sugar solution as a binder to decrease unagreeable feeling of the sweetness on the tongue.

Description

[Detailed Description of the Invention] "Industrial Application Field" This invention utilizes a beet sugar manufacturing process to recover sugar and separate raffinose fractions.
The present invention relates to a method for producing a sweetener that converts necrose directly or contained therein into an oligosaccharide using a transferase and promotes the growth of useful bacteria.

``Prior art'' Raffinose is present in sugar beet used for sugar beet production.
At the sugar beet manufacturing factory, the raffinose that has migrated into the sugar solution is broken down into 7-ucrose and galactose using the enzyme melipiase to increase the yield of sucrose and to prevent raffinose from inhibiting the 5f9 process. In the ion-exchange desalting method, in which various impurities are removed from a sugar solution using an ion-exchange resin, 'a thick juice is roasted with sugar to obtain product sugar, then the A syrup is re-roasted, and the B sugar and B sugar Get Shiratsubu. This B sugar will be dissolved and returned to the concentrated juice process.

B/Shirabu Since this is treated with melibiase, the increased amount of sucrose in B Shirabu is recovered as C sugar by decocting it, then dissolved and returned to the concentrated juice process. In general, raffinose in B/shiratube before melibiase degradation is 8 to 1.
More than 70 g of it is broken down by melipiase and recovered as sucrose, and the rest is discharged together with blackstrap molasses.

On the other hand, Nyucrose generates oligosaccharides by transferases, producing sweet-tasting fructo-oligo shields (Tokuko Sho 5).
9-53834 (see Publication No. 9-53834 fIi)), it is known that inrafinose is produced (see program page 148 of the 77th Japan Society of Gastrointestinal Research in 1985), and the fructooligo shield is used for the growth of bifidobacteria. In addition to what is stated in the above-mentioned Japanese Patent Publication No. 59-53834,
It has been found that the raffinose and inraffinose are also selectively assimilated by Bifidobacteria.

"Problem to be solved by the invention" The inventors first treated B syllabi with melibiase,
More than 70% of the raffinose contained is decomposed into sucrose and galactose, and the sucrose is decanted and recovered in the sugar manufacturing process. 7 Focusing on ucrose, we found that raffinose, which serves as a medium for bifidobacteria, has weak substrate specificity even under conditions where fructosyltransferase converts ucrose in molasses into oligosaccharides, so most of the raffinose remains. Patent application No. 59-126515 for a method for producing a sweetener that converts sucrose in sugar beet into fructooligosaccharide and promotes the growth of bifidobacteria together with raffinose.
However, most of the remaining raffinose in sugar beet molasses was converted into sucrose and galactose through the melibiase decomposition process, so the original B.
/ 10 to 30 of the raffinose content contained in the shirub
There was a drawback that only about % could be used.

This invention eliminates the drawback of poor recovery of raffinose due to conventional decomposition of raffinose with melibiase, recovers high-quality sugar without using melibiase, and recovers raffinose, etc. We conducted research to recover a large amount of useful sugars, and we repeatedly boiled the desalted beet sugar solution to increase the raffinose concentration, and chromatographically separated the 1-separated sugar beet sugar syrup, which was found to be supersaturated with raffinose at room temperature. The raffinose fraction is divided into a raffinose-rich fraction, a high-purity sucrose fraction, and a fraction containing many impurities such as vemain.The high-purity sucrose fraction is returned to the recovery process, and the raffinose fraction is either converted to oligosaccharide using a transferase or left unconverted. The problem was solved by concentrating it.

The desalted beet sugar solution of the present invention is obtained by desalinating sugar beet juice using an anion-cation exchange resin or a membrane, and is usually desalted using an ion exchange resin.

Conventionally, the production of beet sugar from this desalted product is as shown in the process chart of the drawing, by concentrating the purified sugar juice by desalting and decolorizing it to obtain concentrated juice, and then decocting the concentrated juice (A decoction sugar). From this, product sugar is obtained, and the molasses and washing water that have been mixed at this time are used as A-shirubu to again obtain roasted sugar (B-roasted sugar), LB sugar, and B-shirubs. This B sugar is further dissolved and returned to a concentrated juice, which is then roasted in the A sugar roasting process. In addition, conventionally, the raffinose contained in the sugar solution was converted into sucrose by melibiase enzyme and recovered in the B-sill tube, but in the present invention, the raffinose contained in the B-sill tube is not decomposed by melibiase and is recovered by chromatography. The liquid is passed through a column filled with ion exchange resin at 60 to 70°C, and the fraction containing a large amount of raffinose is collected. Raffinose has low solubility at room temperature, and it decreases further when other sugars are dissolved, but it has a solubility of 60-70
At °C, it shows a fairly high @solubility. In the raffinose fraction obtained by the chromatographic separation, raffinose is dissolved in a nuclose solution, and when it is placed under conditions of sucrose and sucrose transition, most of it remains as it is because its substrate specificity is weak.

Furthermore, raffinose itself has a sweetness that is 0.0% sweeter than that of euclose.
Since it is twice as small, if you add other sweeteners,
There is no problem when mixing in solution.

If it is solidified as crystals and used with other sweet ingredients, the solubility will be different when it is added during the day, resulting in an unpleasant sweet taste on the tongue. An effective means is to add powdered sugar as a binder to raffinose when mixing it and granulate it.

"Function" The round roasted sugar syrup used in this invention has been desalted, so it has relatively few impurities, and an analysis example of the compound sucrose/wrap shown by B/lamp in the drawing has a Brix degree of 750.
．． / Knee Clothes Section 52.5.

Raffinose 10.0%, reducing sugar 1.5 parts, betai/8
．． It is 0%. Adjust this to an appropriate concentration and hold at 60-70℃.
When the solution is left in an ion exchange resin column for chromatography overnight, very good separation is achieved and a highly concentrated raffinose solution is obtained.

The ion exchange resin used is Upper Rye) IR-
120, DOWEX 50 WX 6 + DIAION 5K-IA (both trade names) Ca-type strong acidic cation exchange resin or Na-type strong acidic cation exchange resin, especially those with a degree of crosslinking of 4 to 61 and a particle size of 50 to The one with 100 meshes is good. These resins are treated with mW of CaCl2 or the like to form a Ca type, or are converted to a Na type with a solution of NaC, etc., and are filled into a long and narrow resin column. The liquid passing temperature can be 30 to 80°C, but it is preferably 60 to 70°C, which is the sugar refining process B temperature. Then, each fraction is extruded with hot water at the same temperature to extract divided raffinose fractions.

Table 1 shows the results of passing the resin using Ca type DOWEX 50wx6 (trade name).

Table 1 (H) As shown in Table 1 above, sucrose flows out after raffinose, and later, monosaccharides first and then petaine flow out, so if the fractions No. 1 to No. 5, which are rich in raffinose, are collected and classified as raffinose, this #i<71 composition of raffinose division is as follows.

Table 2 (Unknown items are oligosaccharides such as Kesdose and pigments, etc.)
As shown in Table 2 above, the solid content ratio of raffinose is 22.
A solution with a high raffinose content of 4% can be obtained. In addition, in Table 1, fraction Nn6~
Nn8 has a lot of sucrose and raffinose is originally 1
Since it is only 7.8%, this is returned to the diluted juice during the process,
Fractions N n 9 to No. 13 can be used as petaine-containing fractions for the production of petaine.

This is the raffinose-containing solution! It may be concentrated and used as a sugar source sweetener selected for Bifidobacterium growth, or it may be used as granulated sugar by precipitating raffinose after concentration and mixing powdered sugar with it to form granulated sugar. In this case, it is preferable to add reducing sugars such as molasses and high-fructose sugar as a binder during mixing.
We investigated the discomfort of the sweetness of 1 granulated sugar when granulated with and without reducing sugar.
When tested by 0 panelists, the results are as shown in Table 3.

Table 3 A raffinose supersaturated solution containing the components shown in Table 2 preferably contains/Uculose is converted into an oligosaccharide using a transferase to produce a sweetener containing a large amount of bifidobacterium-proliferated carbohydrate source. The transferase used is an enzyme that produces oligosaccharides from 7-ucrose or a bacterial cell containing the enzyme, such as fructosyltransferase or Aureobasidium pullulans AHV9549 that has the ability to produce the enzyme.
Bacterial strain/Yukos 20%, NaN031% +M
gSO4・7H200.05%, 2HPO40.5%
, corn staple liquor 2q6. p containing urea 4t
Aeration culture was carried out in H6 medium, and the bacterial cells were centrifuged and washed.9
Then, it was thoroughly mixed in a sodium thialginate solution, and
This is enzyme-immobilized bacterial cells that are made into granules by being added dropwise to a calcium chloride solution. The immobilized bacterial enzyme produced in this way usually has a fructonortransferase activity of 20 to 40%.
Unit/■Dry matter.

The reaction between the raffinose supersaturated solution and the enzyme can be carried out in a fixed bed method or a fluidized bed method. For example, a jacketed column with an inner diameter of 10 m and a height of 50 crn is filled with 3 tons of the immobilized bacterial enzyme. The second pH was adjusted to 5.
A supersaturated raffinose solution with the composition shown in the table was heated at 60-70℃.
at a flow rate of 0.2 volume per bacterial enzyme volume (600 CC/H
) to pass the liquid upward from the bottom of the column. Table 4 shows the average composition of the reaction solution when this was continued for 30 days.

Table 4 (H) Means fructooligosaccharides with different raffinose contents.

As is clear from Table 4, most of the raffinose present in the raffinose supersaturated solution of the treated solution remains, and when the produced fructooligosaccharide is added, 59.7% of the total solid content is the selective sugar that promotes the growth of bifidobacteria. It is a sweetener that contains oligosaccharides that act as a quality source. In other words, the oligosaccharide-containing sweeteners in Table 4 do not convert into monosaccharides even if they are placed in artificial gastric fluid (containing 0.2% salt and 0.32% pepsin [adjusted to 5 Hl]) and kept at 37°C. The rate of decomposition is small, and after retention, it can be neutralized to produce Bifidobacterium longum (B
When Bifidobacterium such as Bifidnbacterium Lnngum is cultured, it shows extremely good growth.

The sweetener of this invention may be used as is.

It may also be mixed with other foods. Furthermore, it may be used in combination with other sugars having a bifidus effect.

Next, an example of implementation will be described.

"Example 1" Inner diameter 87 crn, height 250 (77+, resin layer height 170 crn)
250 to 10 grains in a jacketed stainless steel column
0 mesh Ca type DOWEX 50wx4 (product name)
125 tons of B syrup-adjusted sugar solution filled with 1 m' of resin and produced by the process shown in 9 drawings was heated to a temperature of 60'CS V O, 6.
and extruded with warm water at 60°C to obtain a raffinose sugar solution. Next, this raffinose fractionated sugar solution was subjected to Bx
After concentrating to pH 60 and adjusting the pH to 5, the 5 Kf was placed in a 20 volume tank and heated to 55°C.

Add fructosyltransferase to this at 30 units/W.
q Aureopa7 deum pullulans AHU9 including dry matter
549 alginate Cal/Rum entrapped immobilized bacterial cells 500
2 was added and the mixture was stirred and maintained at that temperature for 5 hours to react.

After the reaction is completed, the bacterial cells and sugar solution are separated by centrifugation, and the bacterial cells are returned to the same tank and the enzyme treatment reaction is repeated 10 times.
A processing solution having a solid common ratio of 60.5 and the following composition was obtained.

Table 5 Next, the enzyme-treated solution shown in Table 5 was reduced to Bx75 to obtain a @ solution containing raffinose with an oligosaccharide purity of 57.8%.

This sugar solution was a sweetener suitable for promoting the growth of bifidobacteria and had a mild sweet taste.

"Example 2" The raffinose supersaturated sugar solution obtained by the chromatographic separation in Example 1 was concentrated to Bx75 and then cooled to crystallize raffinose, which was then centrifuged to obtain raffinose crystals.

After drying this raffinose, add an equal amount of powdered sugar and 10% of the total weight of high fructose sugar and mix well. After granulation, a fluidized bed dryer (MDB-1 manufactured by Fuji Powder Co., Ltd.
000 type).

It was dried at 75°C for 10 minutes. This granulated sugar had a mild sweet taste and was suitable as a sweetener for the growth of bifidobacteria.

``Effects'' This invention chromatographs the raffinose concentrated in the beet sugar production process and returns the sucrose separation to the production process, so the troublesome C-boiled sugar can be omitted.

In addition, a large amount of raffinose can be recovered from the divided raffinose fraction without requiring the conventional treatment step using melibiase. In addition, ucrose, which is included in the raffinose category, can be efficiently produced with oligosaccharides and raffinose using a transferase to produce a high-quality sweetener that has a bifidobacteria growth effect.

[Brief explanation of drawings]

The drawing is a process chart showing a comparison between the conventional method and the water droplet method. drawing Conventional law Main law Thick soup Thick soup ↓　　　　↓ Made of Molasses Procedural amendment (formality) February 1986? Day

Claims (4)

[Claims] (1) Repeated pre-saccharification of the beet sugar solution desalted using an ion exchange resin, and chromatographic separation of the separated pre-saccharide syrup for the base material. The high-purity sucrose fraction is returned to the recovery process, and the raffinose fraction contains a bifidobacteria-propagated carbohydrate source that can be converted into oligosaccharides using a transferase or concentrated without conversion. A method for producing a sweetener. (2) The method for producing a sweetener containing a bifidobacteria-proliferated carbohydrate source according to claim 1, wherein the transferase is fructosyltransferase or β-galactosidase. (3) The sugar solution desalted using an ion exchange resin is repeatedly pre-saccharified, and the separated pre-saccharide syrup is chromatographically separated, and a segment with supersaturated raffinose at room temperature, a segment with high purity sucrose, and a segment with a large amount of petaine are separated. The high-purity sucrose fraction is returned to the recovery process, and the raffinose fraction is either converted to oligosaccharide using a transferase or concentrated without conversion, and then the raffinose-containing oligosaccharide is collected and the resulting sugar is A method for producing a sweetener containing a bifidobacteria-proliferating carbohydrate source, which comprises mixing with powdered sugar and granulating the mixture. (4) A method for producing a sweetener containing a bifidobacterium-propagated carbohydrate source according to claim 3, which comprises adding a reducing sugar solution as a binder when mixing raffinose-containing sugar and powdered sugar.