JPS61104800A - Production of powder containing ractulose crystal - Google Patents

Abstract

(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

Detailed Description of the Invention [Industrial Application Field 1] The present invention relates to a method for producing lactulose crystal-containing powder,
More specifically, the present invention relates to a method for producing two lactulose crystal-containing powders from a lactulose-containing water W3 solution. Lactulose is a useful disaccharide that is widely used in the fields of medicine, food, etc. as bifidus 7T. [Joura's technology] Attempts to crystallize and separate lactulose from a lactulose-containing aqueous solution have been made for a long time.
of American Chemical 5
ociety, Volume 5 2! 210il, 1930)
, WhisLIer et al. (edited by R, L. Wbistler et al. + Methods in C
arbohydrrrLeChemistry+ 1 volume *325TLAcademic Press+Ne
w York and London, 196
2 years), established (Nyufukyo Materials, Vol. 22, No. 2, p. 3, 19
(1972) describes it in detail. However, although these methods are effective in the laboratory, they are not suitable for industrial use because the process is complicated and they use tutanol, which is harmful to the human body, and cannot be completely removed. has the disadvantage that it cannot be put into practical use. As described above, since it is extremely difficult to crystallize lactulose, conventional methods have been used industrially to powderize an aqueous F# solution containing Fukutulose by spray drying, etc., without crystallizing it. ing. Methods for producing lactulose-containing powder from a lactulose-containing aqueous solution with a positive lactulose content include grain flour (m Publication No. 40-861), konjac powder (Japanese Patent Publication No. 49-44331), and protein (Japanese Patent Publication No. 49-44331).
A method of adding a drying aid such as -44332) to the aqueous solution and drying it, and a method of freeze-drying the aqueous solution (Japanese Patent Laid-Open Publication No. 49-49-
54556) is known. However, among these methods, methods using drying aids have the disadvantage that grain flour, konjac powder, and protein are contained in the final powder, and methods that do not use earthy drying aids result in lower yields and There are disadvantages such as an increase in the amount of powder produced, and furthermore, although the moisture content of the powder obtained by any of the above methods is low, it is highly humid and does not absorb moisture in a normal indoor environment. The disadvantage is that it tends to solidify. Therefore, when the powder obtained by these methods is processed such as packaging or tabletting, there is an inconvenience that the powder must be handled indoors with low humidity. There were many problems with packaging. As a method to solve these drawbacks of the conventional method, a treatment method in which a special crystallization treatment is performed using ethanol has recently been published. Specifically, Japanese Patent Publication No. 56-39200 describes a method in which an aqueous solution of lactulose is made into an amorphous dry powder by spray drying, etc., and then further treated with ethanol to produce a lactulose powder with low hygroscopicity. Further, JP-A No. 57-102200 describes a method in which ethanol is added to a concentrated solution obtained by adding glycerin or propylene glycol to an aqueous lactulose solution to separate and dry solid matter. However,
The method of No. 9200 not only requires an extra operation to turn the aqueous solution of lactose into a dry powder, but also requires strict control of the water content using anhydrous ethanol, which is disadvantageous in terms of cost (and cost). *However, the method of JP-A-57-102200 has the disadvantage that the glycerinone or propisine glycol used remains in the powder, albeit in a small amount, resulting in a different taste. [Problems to be Solved by the Invention] The present invention improves the drawbacks of the conventional lactulose pulverization method as described above, and provides a method for advantageously producing a high-quality lactulose crystal-containing powder that is difficult to sip. That is, until now, there has been no report on obtaining lactulose crystals from an aqueous system, but as a result of various studies conducted by the present inventor on methods for producing 91R lactulose crystals from an aqueous system using a kneading method, it was found that lactulose crystals can be obtained under specific conditions. That is, the solid content concentration of the lactulose concentrate after adding crystal seeds was adjusted to 94 to 98% by 11stL,
Furthermore, it has been found that when ripening after kneading is carried out at 35 to 70 DEG C., crystallization of Fukutsu-A-su progresses well and a crystal-containing solidified product is produced in a relatively short period of time. [Structure of the Invention] The present invention was completed based on the above-mentioned findings, and is based on the FI4J! 60～
While maintaining the temperature at 110°C, add crystal seeds to adjust the final solid concentration of the concentrate to 94-98%, knead it, and then maintain the kneaded product at 35-70°C if desired. SO1! is a powder containing lactulose crystals, which is produced by aging and then pulverizing the obtained solidified product. It's a method. The lactulose aqueous solution used in the present invention has a lactulose content of 60% or more, preferably 80% or more in solid content. 52
-91 method)). Lactulose aqueous solutions prepared in this way often contain a small amount of lactose in addition to the main component, lactulose.
However, it contains impurities such as lactose. Concentration of the Laflami aqueous solution is carried out according to the conventional method, but as mentioned above, the lactulose aqueous solution contains various impurities, and these change in quality and color when heated, so strong heating is performed during concentration. In addition, increasing the S# of the lactulose aqueous solution to 94% or more, especially 95% or more is not only extremely disadvantageous in terms of thermal efficiency, but also technically difficult as described above. Therefore, in the present invention, the lactulose aqueous solution is usually
After concentrating to about 95%, a required amount of crystal seeds is added thereto to increase the solid content concentration. As crystal seeds, not only 6-purity lactulose crystals that are commercially available as reagents, but also commercially available crystal-containing powder products of relatively low purity (75% purity) can be used. It is also possible to use a crystal powder crystallized from an organic solvent such as 1, methanol, or ethanol, or a powder containing Fuku gamma cous crystals obtained in the present invention as the large crystal seed. The amount of crystal seeds added depends on the degree of concentration of the resulting concentrate (solid content concentration) and the proportion of 2-cutolite in the solid content (lactose a).
- The amount is increased or decreased as appropriate depending on the purity. That is, in general, the higher the lactulose purity in the solid content, the smaller the amount of crystal seeds added is required, and conversely, the lower the lactulose purity, the more it is necessary to add the crystal seeds. *
In addition, in the present invention, the final solid concentration of the concentrate is at least 94 to 98%, preferably 95 to 9%, with the addition of crystal seeds.
It is necessary to set it to 7%. More specifically, when the lactulose purity of the concentrate is 95%, it is about 1% or more of the concentrate, when the purity is 80%, it is about 10% or more of the concentrate, and when the purity is 60%, it is about 1% or more of the concentrate. Approximately 50% or more, and the final l! L-form separation concentration record 1t! For example, if the purity of lactulose in the solid content is 95.
% and in the case of a concentrate with a solid content concentration of 96%, it is sufficient to add about 1% of crystal seeds, but even with the same lactulose purity, the solid content concentration is 93.5%. In a concentrate, the amount of crystal seeds required is 1096 or more.In addition, in a concentrate where the lactulose purity in the solid content is 80% and the solid content concentration is 94%, the amount of crystal seeds added is required to be 10% or more. , furthermore, the lactose purity in the solid content is 60%,
In the case of a concentrate having a solid content concentration of 94.5%, it is necessary to add about 50% or more of crystal seeds. Integration of the concentrate is carried out until the crystal seeds added are sufficiently distributed throughout the concentrate while maintaining the concentrate at a relatively high temperature at which melting of the added crystal seeds does not occur and browning of the concentrate does not occur. . The kneading means can be hand kneading, but in order to perform sufficient kneading, a kneading machine is usually used, preferably a kneading machine of a type that can be lightened by inserting -8 air into the kneaded material. A method of kneading is used. Although it depends on the purity of S-concretion,
It is usually preferable to knead at 60 to 110°C, more specifically, 85 to 110°C if the lactulose purity of the concentrate is 95% or more, and 65 to 90°C if the purity is 80%.
When the purity is 60%, a method of kneading at 60 to 75°C is usually used. After kneading, the kneaded product is heated to a specific temperature (i.e. 35~
It is preferable to hold the lactulose at a temperature of 70°C and ripen it so that the crystals are fully separated.In other words, the crystallization of lactulose after synthesis is extremely slow at room temperature, and as the temperature increases, it crystallizes. Therefore, in the present invention, a method is usually used in which ripening is carried out at a relatively high temperature at which coloration does not occur much, that is, at about 35 to 70°C. After the crystallization has sufficiently progressed, the obtained solidified product containing lactulose crystals is pulverized using a conventional pulverizer. In addition, if the moisture content of the obtained powder is high and the fluidity is poor, it is preferable to further perform a drying treatment [Advantage 1 of the Invention As described above, in the method of the present invention,
No organic solvent is used to prepare the crystal-containing powder, and the manufacturing process is much shorter than that of conventional methods.Furthermore, the crystal-containing powder obtained is more hygroscopic and breathable than the conventional method. Therefore, this method is extremely useful as a method for powdering Fukutoose. Next, the results of testing the hygroscopicity of the Fukutsu-A-s crystal-containing powder produced by the method of the present invention (the powder of the present invention) will be shown. Test Wk1 Each sample powder was exposed to various humidity at 27℃ for 24 hours.
This was done by visually observing changes in the external shape while hiding the specimen. As a sample, the powder of the present invention was used as Example 1.2.
．． The powders obtained in Examples 3 and 6 were used, and as a control powder, a powder obtained by simply concentrating, solidifying, and then pulverizing the same lactulose aqueous solution used in Example 2 was used. The results are shown in Table 1. As is clear from mis, at 27℃ salinity, 1Il at 24 hours.
When left alone, the control powder already solidifies at 30% humidity, whereas the lactulose crystal-containing powder according to the present invention shows no change even at 60% humidity, indicating that it is a very stable powder. I understand. Trial Wk2 The powder obtained in Example 2 was used as the inventive powder, and the same control powder as used in Test 1 was used as the control powder.
Each sample was exposed to the atmosphere at a temperature of 27° C. and a humidity of 50%, and the moisture absorption rate was measured over time. The result is lJ in Figure 1.
i It is shown in the wet curve diagram. As is clear from FIG. 1, the powder of the present invention does not absorb moisture at all after one day and reaches an equilibrium state, indicating that it is extremely stable compared to the control powder. [Actual Examples] The present invention will be explained in more detail by referring to Examples below. Example 1 Lactulose aqueous solution [(solid content concentration 60%, lactulose purity 95%, lactose 4%, lactose 1%) 1 kg
Concentration was performed at 0°C to obtain a concentrate with a solid content of 96%. Transfer the obtained concentrate to a tray and keep it warm at 110°C.
Lactulose crystal fine powder 101r was added as a crystal seed and thoroughly stirred and kneaded (combined for 10 minutes using a food-grade egg whisk).Next, this kneaded product was aged at 70°C overnight to obtain a mixture. The solidified product was pulverized into powder using a pulverizer.Then, this powder was dried at 60° C. overnight to obtain 550 gr of lactulose crystal-containing powder. This powder was a white powder with low hygroscopicity and high fluidity at s, p, 163 to 165°C. Example 2 Aqueous sucrose solution (solid content concentration 68%, lactulose purity 80%, lactose 7%, lactose 13%) was concentrated at 60°C to obtain a concentrate with a solid content concentration of 94%. Next, this MS material was transferred to a tray, and 0.65 kg of crystal seeds was added while keeping the temperature at 90°C, and thoroughly kneaded. The resulting solidified product was pulverized using a pulverizer to form a powder. Next, this powder was dried at 60° C. overnight to obtain a lactulose crystal-containing powder. The melting point of this powder was 151 to 152°C, and it was a stable white powder with low hygroscopicity. Example 3 Lactulose aqueous solution (solid concentration 68%, lactulose purity 80%, milk 1s 7%, lactose 13%) 0.5
Next, this concentrate was concentrated at 60 to 100°C to obtain a concentrate with a solid content concentration of 93%.Then, this concentrate was kneaded using a tfiI Irie Shokai Co., Ltd., BENCII KNEADER%Mode.
1PNP - Transferred to January, crystal seeds (
0.34 of the powder obtained in Practical Example 2 was added and kneaded in 5 volumes.Then, this kneaded product was transferred to a tray and aged at 50°C for 2 days, and the obtained assimilate was crushed. A powder was obtained. This powder was further dried at 50° C. overnight to obtain a powder containing lactulose crystals. The melting point of this powder was 151.5°C, and it was a stable white powder with low hygroscopicity. Implementation f14-8 Powderization of the lactulose aqueous solution was carried out according to the method of Example 3, except that the concentration, amount of crystal seeds added, kneading temperature, and VH mixing time were changed as shown in Table 2. A stable lactulose crystal-containing powder with low humidity and a melting point as shown in Table 2 was obtained. Example 9 Lactulose aqueous solution (solid content concentration 50%, lactulose purity 60%, lactose 35%, lactose 5%) lkf was concentrated at 80°C to obtain a concentrate with a solid content concentration of 94.7%. Ta. This concentrate was mixed with a kneading machine [Irie Shokai Co., Ltd., BENCHK]
Transfer to NEADER, Model PNP till, add 250g of crystal seeds while keeping at 65℃,
No.5 Question 1 Next, transfer this mixture to a tray and mix it for 50 minutes.
After ffi incubation at ℃ for 2 days, the obtained solidified product is pulverized with a pulverizer to form a powder. Furthermore, this powder was dried at 50°C overnight,
A powder containing lactulose crystals was obtained. This powder was a white powder with s, p, 139-133°C. Jitsukai■O Lactulose aqueous solution (solid concentration 68%, lactulose purity 8096, lactose 7%, 〃Tikudose 1396>0.
5klB was concentrated at 60-100°C to a solid content concentration of 94.
A 3% concentrate was obtained.Then, this concentrate was passed through a kneading machine (c
(Same as ASEN3) and crystallize while keeping warm at 75℃!
11 (powder obtained in Example 2) was added to 0.17, and 5.
After kneading for a minute, this kneaded product was cooled, and the obtained solidified product was pulverized to obtain a powder containing lactulose crystals. This powder is a white powder with a melting point of 135-138°C.

[Brief explanation of the drawing]

The PIS 1 diagram is a moisture absorption curve diagram when the Fukutsu-A-S crystal-containing powder (invention powder) and the control powder were exposed to the atmosphere at a temperature of 27° C. and a humidity of 50%.

Claims (1)

[Claims] 1. Concentrate an aqueous lactulose solution containing 60% or more of lactulose in solid content, and heat the resulting concentrate at 60 to 110°C.
lactulose crystal-containing powder, which is characterized in that the final solid content concentration of the concentrate is adjusted to 94 to 98% by adding crystal seeds to the powder, kneading the concentrate, and pulverizing the obtained solidified product. Production method. 2. The method according to claim 1, characterized in that a lactulose aqueous solution containing 80% or more of lactulose in solid content is used. 3. Method according to claim 1 or 2, characterized in that the final solid concentration of the concentrate is adjusted to 95 to 97%. 4. Lactulose aqueous solution containing 60% or more of lactulose in solid content. Concentrate the obtained concentrate at 60-110℃
The final solid concentration of the concentrate was adjusted to 94 to 98% by adding crystal seeds while maintaining the temperature at A method for producing a powder containing lactulose crystals, which comprises pulverizing the obtained solidified product. 5. The method according to claim 4, characterized in that an aqueous lactulose solution containing 80% or more of lactulose in solid content is used. 6. The method according to claim 4 or 5, characterized in that the final solid concentration of the concentrate is adjusted to 95 to 97%.