MIXED SUGAR GRANULAR POWDER AND METHOD FOR PREPARING SAME
20180179604 ยท 2018-06-28
Assignee
Inventors
- Go-Eun Kim (Gwangju, KR)
- Sung Won PARK (Daejeon, KR)
- Su Youn Lim (Suwon-si, KR)
- Hye Jung KIM (Daejeon, KR)
- Chong Jin PARK (Daejeon, KR)
- Kang Pyo Lee (Seoul, KR)
Cpc classification
C13B50/00
CHEMISTRY; METALLURGY
C13K13/00
CHEMISTRY; METALLURGY
International classification
C13K13/00
CHEMISTRY; METALLURGY
C13B50/00
CHEMISTRY; METALLURGY
Abstract
The present invention relates to a granular form of mixed saccharide composition comprising a mixed saccharide containing psicose as a main ingredient and a method for preparing the same, and more particularly to a granule of a mixed saccharide containing psicose with improved sweetness quality and physical properties and a method for preparing the same.
Claims
1. A mixed saccharide granule comprising; (a) a first saccharide powder containing psicose; and (b) a second saccharide powder which has 30 to 170 of a ratio of an average particle diameter, based on 100 of an average particle diameter of the first saccharide powder, and is at least one selected from the group consisting of monosaccharides other than psicose and disaccharides, wherein hygroscopicity of the mixed saccharide granule is 90 or less, based on 100 of hygroscopicity of psicose powder.
2. The mixed saccharide granule of claim 1, wherein the flowability of the mixed saccharide granule is 120 to 200, based on 100 of the flowability of the psicose powder.
3. The mixed saccharide granule of claim 1, wherein the mixed weight ratio of the first saccharide powder and the second saccharide powder (the first saccharide powder:the second saccharide powder) is 70:30 to 5:95.
4. The mixed saccharide granule of claim 1, wherein the average particle diameter of the mixed saccharide granule is 100 to 250, based on 100 of the average particle diameter of the first saccharide powder.
5. The mixed saccharide granule of claim 1, wherein the average particle diameter of the first saccharide powder is 50 to 300 m, and the average particle diameter of the second saccharide powder is 50 to 700 m.
6. The mixed saccharide granule of claim 1, wherein the second saccharide powder is at least one saccharides selected from the group consisting of sucrose, lactose, maltose, galactose, tagatose, xylose, mannose, allose and fructose.
7. The mixed saccharide granule of claim 1, wherein the mixed saccharide granule is prepared by mixing and drying the first saccharide powder and the second saccharide powder, following the granulation.
8. The mixed saccharide granule of claim 7, wherein mixing and drying are carried out in a fluidized bed granulator.
9. The mixed saccharide granule of claim 1, wherein the mixed saccharide granule further comprises a binding agent of saccharide powders.
10. The mixed saccharide granule of claim 9, wherein the binding agent is one or more kinds selected from the group consisting of water, C.sub.1-C.sub.6 alcohol, aqueous solution of C.sub.1-C.sub.6 alcohol, maltodextrin, indigestible maltodextrin, Hydroxypropyl methylcellulose (HPMC) and starch.
11. The mixed saccharide granule of claim 9, wherein the mixed saccharide granule comprises 0.1 to 5% by weight of the binding agent in the total weight of the granule.
12. The mixed saccharide granule of claim 1, wherein the psicose is provided by a mixed saccharide which comprises 1 to 99.9 parts by weight of psicose based on 100 parts by weight of the total solid content of the mixed saccharide and further comprises at least a saccharide selected from the group consisting of fructose, glucose and oligosaccharide.
13. A method for preparing a mixed saccharide granule comprising, preparing a mixed saccharide granule by granulating (a) a first saccharide powder containing psicose; and (b) a second saccharide powder which has 30 to 170 of a ratio of an average particle diameter, based on 100 of an average particle diameter of the first saccharide powder, and is at least one selected from the group consisting of monosaccharides other than psicose and disaccharides, wherein an average particle diameter of the mixed saccharide granule is 100 to 200, based on 100 of an average particle diameter of the first saccharide powder, and hygroscopicity of the mixed saccharide granule is 90 or less, based on 100 of hygroscopicity of psicose powder.
14. The method for preparing a mixed saccharide granule of claim 13, wherein the granulating step is carried out by adding a binding agent.
15. The method for preparing a mixed saccharide granule of claim 13, wherein the granulating step is carried out by mixing the first saccharide powder and the second saccharide powder and hot air drying at a temperature in the range of 40 to 70 C.
16. The method for preparing a mixed saccharide granule of claim 13, wherein the granulating step is carried out by fluidizing the first saccharide powder and the second saccharide powder in a fluidized bed granulator with spraying a binding agent.
17. The method for preparing a mixed saccharide granule of claim 16, wherein dry air provided to the fluidized bed granulator is 20 to 50% RH, 40 to 70 C. of temperature and 30 to 150 m.sup.3/h of pressure.
18. The method for preparing a mixed saccharide granule of claim 13, wherein the mixed weight ratio of the first saccharide powder and the second saccharide powder (the first saccharide powder:the second saccharide powder) is 70:30 to 5:95.
19. The method for preparing a mixed saccharide granule of claim 13, wherein a binding agent is added so that the content of the binding agent in the total weight of the mixed saccharide granule is 0.1 to 5% by weight.
20. The method for preparing a mixed saccharide granule of claim 14, wherein the binding agent is one or more kinds selected from the group consisting of water, C.sub.1-C.sub.6 alcohol, aqueous solution of C.sub.1-C.sub.6 alcohol, maltodextrin, indigestible maltodextrin, Hydroxypropyl methylcellulose (HPMC) and starch.
Description
BRIEF DESCRIPTION OF DRAWINGS
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DETAILED DESCRIPTION OF THE EMBODIMENTS
[0060] The present invention will be described in more detail by the following examples, but it is not intended to limit the protection scope of the present invention by the following examples.
PREPARATIVE EXAMPLE 1
Preparation of Psicose
[0061] 1-1: Preparation of a Strain Producing Psicose
[0062] An encoding gene of a psicose epimerase derived from Clostridium scindens (Clostridium scindens ATCC 35704) (DPE gene; Gene bank: EDS06411.1) was synthesized as a modified form of polynucleotide by optimizing for E. coli and called CDPE. The polynucleotide optimized for E. coli (SEQ ID NO: 2) and sod promoter and T7 terminator obtained from pET21a vector were obtained as each template through PCR, and these were linked as one template by overlap PCR method and cloned into pGEM T-easy vector through T-vector cloning, thereby confirming sod promoter (SEQ ID NO: 1), optimized CDPE sequence (SEQ ID NO: 8) and a sequence of a polynucleotide comprising T7-terminator.
[0063] The entire confirmed polynucleotide was inserted into the same restriction enzyme site of an expression vector pCES208 (J. Microbiol. Biotechnol., 18:639-647, 2008) using restriction enzymes NotI and XbaI(NEB), and a recombinant vector pCES208/psicose epimerase (pCES_sodCDPE) was prepared. The cleavage map of the prepared recombinant vector (pCES_sodCDPE) was shown in
[0064] Corynebacterium glutaricum was transformed with the prepared recombinant vector (pCES_sodCDPE) plasmid using electroporation. Colonies were picked and inoculated in 4 ml of LB medium (tryptone 10 g/L, NaCl 10 g/L, yeast extract 5 g/L) supplemented with Kanamycin at a final concentration of 15 ug/ml, and then cultured for approximately 16 hrs at the culture conditions of 30 C. and 250 rpm. Then, 1 ml of the culture was collected and inoculated in 100 ml LB medium comprising 15 ug.ml of Kanamycin, and the culture was continued for over 16 hrs.
[0065] After lysis of cells cultured using beadbeater, only supernatant is obtained and mixed with a sample buffer as 1:1, and then heated at 100 C. for 5 minutes. The prepared samples were subjected to electrophoresis on a 12% SDS-PAGE gel (composition: running gel3.3 ml H2O, 4.0 ml 30% acrylamide, 2.5 ml 1.5M Tris buffer (pH 8.8), 100 l 10% SDS, 100 l, 10% APS, 4 l TEMED/stacking gel1.4 ml H2O, 0.33 ml 30% acrylamide, 0.25 ml 1.0M Tris buffer (pH 6.8), 20 l 10% SDS, 20 l 10% APS, 2 l TEMED) at 180V for approximately 50 minutes, and the protein expression was confirmed.
[0066] After the expression of CDPE was confirmed on the SDS-PAGE gel, His-tag purification was proceeded using Ni-NTA resin for accurate measurement of expression level, and the expression rate was calculated using a calculation formula (expression rate(%)=(Purified protein(mg)/Total soluble protein(mg))100). The prepared transformed Corynebacterium glutaricum produced 16.62 mg of the total water-soluble proteins and 1.74 mg of purified enzyme proteins.
[0067] 1-2: Preparation of Psicose Syrup
[0068] In order to prepare psicose from fructose using the recombinant strain producing psicose epimerase obtained from Preparative Example 1-1, cells were collected by centrifugation in the strain culture. Then, the cell suspension was treated with 0.05% (v/v) of en emulsifier (M-1695) in a final volume and treated at 35 C. (5 C.) for 60 minutes. The microbial cells in which the reaction was completed were collected after the supernatant comprising the emulsifier was removed again using a centrifuge.
[0069] For the preparation of immobilized beads, the collected microbial cells were mixed with D.W. to a final microbial cell concentration of 5% (v/v), and 4% (v/v) of alginic acid dissolved in water and 5% (v/v) of the collected microbial cells were mixed at 1:1, and it was refrigerated at 4 C. to remove bubbles generated during mixing. The refrigerated mixture solution was injected through Neddel (inner diameter 0.20 to 0.30 mm) and formed into a droplet shape, and dropped by weight, and the dropped mixture solution was dropped into a previously prepared 100 mM calcium chloride (CaCl.sub.2) solution and cured, and spherical or elliptical beads (diameter 2.0 to 2.2 mm) were formed. The formed beads were soaked in a 100 mM calcium chloride solution and mixed evenly by a stirrer so as to be further cured.
[0070] After all the mixture solution was injected, the beads were further cured while being refrigerated for 4 to 6 hrs, and then cured for approximately 6 hrs in a refrigerated state by replacing a new 100 mM calcium chloride solution. After beads completely cured were skimmed and moisture was completely removed, water was added 3 times as much as the volume of the beads and then it was stirred for 10 minutes, and the calcium chloride solution was removed by treating the beads with this process 3 times.
[0071] After completely removing water from the washed beads for manganese soaking, 40 brix (%) the reaction substrate comprising 10 mM manganese was added at 3 times volume of bead volume, and then stirred for 10 minutes, and it was replaced with the reaction substrate comprising 10 mM manganese by repeating this treatment 3 times or more. The reaction substrate was adjusted to pH 6.8 to 7.2 with 3N NaOH, and liquid fructose or crystalline fructose can be the substrate depending on the kind of product. The beads completely soaked have a reduced diameter of approximately 1.6 to 1.8 mm and its strength was also increased. After removing the substrate of beads completely soaked, they were filled in an immobilized reaction column and then used for the production of a psicose syrup.
[0072] <Immobilized Column Reaction Conditions>
[0073] Reaction temperature: internal temperature of the column jacket 50 C.
[0074] Substrate flow rate: 0.5 SV (space velocity L.h.sup.1)
[0075] Reaction substrate: crystalline fructose 40 brix, pH 6.8 to 7.2,
[0076] Bead preparation: 2.5% (w/w) microbial cells, 2% (w/w) alginic acid mixture and 10 mM Mn2.sup.+ soaking
[0077] To the immobilized reaction column, a raw material whose raw material solution comprised 75% of solid and the fructose content was 92 parts by weight when the total solid content was 100 parts by weight was provided, thereby preparing a psicose syrup. The 25(w/w) % psicose syrup in which the weight ratio of glucose:fructose:psicose:oligosaccharide is 6:67:25:2 was collected from the reaction solution.
[0078] 1-3: Preparation of Psicose Powder
[0079] In order to remove impurities such as color and ion components, the psicose syrup obtained from Preparative Example 1-2 was passed through at a rate of 2 times (once or two times) volume of the ion exchange resin per hour in a column at the room temperature which was filled with resin in which anion exchange resin and cation and anion exchange resin were mixed and desalted, and then a high-purity psicose solution was separated and collected using chromatograph which was filled with an ion exchange resin of the calcium (Ca.sup.2+) type. The high-purity psicose syrup was concentrated at a concentration of 82 Bx (%, w/w) (80 to 83 Bx), and cooled from 35 C. (35 C. to 40 C.) of temperature to become a supersaturated state to 10 C. (10 to 15 C.) of temperature gradually, thereby forming crystals. The psicose crystals obtained in the crystallization step, in which psicose crystal seed was not added, were collected by drying after removing mother liquor by centrifugal dehydration and washing crystals with cooling water.
[0080] The average particle size of the obtained psicose crystal powder was 237 m, and its range of particle diameter was distributed in 74 to 428 m, and the crystal structure had a long rectangular parallelepiped shape with an orthorhombic system. The widthlength diameter ratio of the rectangular parallelepiped crystal is 14 on average, and has a diameter in the range of 11.5 to 6.9. The scanning electron micrograph (SEM) photograph of the psicose crystal and the stereoscopic microscope photograph (400 magnification) of the psicose crystal were shown in
EXAMPLE 1
Preparation of Mixed Granule of Psicose and Glucose
[0081] 1-1: Use of Anhydrous Glucose with 295 m of the Average Particle Size
[0082] After mixing 150 g of each psicose powder prepared in Preparative Example 1-3 and anhydrous glucose powder in which the average particle size was 295 m to be the weight ratio (w/w) of 1:1, the powder was put into a fluidized bed granulator dryer (FBS, manufactured by HTTLIN, Germany) set at the conditions of InLet temperature 50 C., OutLet temperature 40 C., and Air pressure 30 m.sup.2/h, thereby preparing a granule and drying. At this time, in order to from a granule well, the binding solution was sprayed for 15 minutes at a speed of 10 rpm as much as 10 to 20% volume of the total weight of the total mixed powder weight with a fermentation alcohol having a purity of 95% or more. The alcohol was advantageous in that it was volatilized when sprayed and did not exist in the powder, so it did not affect the content. After the internal temperature was slowly cooled to below 30 C. when all alcohols were sprayed, the granular powder was taken out of the equipment and collected. A stereoscopic microscope photograph (400 magnification) of the obtained mixed granular powder of psicose and anhydrous glucose was shown in
[0083] 1-2: Use of Hydroglucose with 261 m of the Average Particle Size
[0084] After mixing 150 g of each the psicose powder prepared in Preparative Example 1-3 and a hydroglucose in which the average particle size is 261 m in a ratio of 1:1 (w/w), a granule was prepared in substantially the same manner as Example 1-1.
EXAMPLE 2
Preparation of Mixed Granule of Psicose and Sugar
[0085] 2-1: Use of Powdered Sugar with 72 m of the Average Particle Size
[0086] After mixing 150 g of each the psicose powder prepared in Preparative Example 1-3 and a powder sugar (which is prepared by pulverizing sugar and is disclosed in Table 1) in which the average particle size is 72 m in a ratio of 1:1 (w/w), a granular powder was prepared in the same manner as Example 1.
[0087] 2-2: Use of Ultra-Finely Granulated Sugar with 230 m of the Average Particle Size
[0088] After mixing 150 g of each the psicose powder prepared in Preparative Example 1-3 and a ultra-finely granulated sugar(caster sugar) in which the average particle size is 230 m in a ratio of 1:1 (w/w), a granular powder was prepared in the same manner as Example 1.
[0089] 2-3: Use of Finely-Granulated Sugar with the Average Particle Size is 392 m
[0090] After mixing 150 g of each the psicose powder prepared in Preparative Example 1-3 and a finely-granulated sugar in which the average particle size is 392 m in a ratio of 1:1 (w/w), a granular powder was prepared in the same manner as Example 1.
[0091] 2-4: Use of Granulated White Sugar with 684 m of the Average Particle Size
[0092] After mixing 150 g of each the psicose powder prepared in Preparative Example 1-3 and a granulated white sugar(general sugar) in which the average particle size is 684 m in a ratio of 1:1 (w/w), a granular was prepared in the same manner as Example 1.
EXAMPLE 3
Preparation of Mixed Granule of Psicose and Sugar using Binding Agent
[0093] In order to form granules between powder particles evenly, as binding agents, DE12 maltodextrin, natural water-soluble dietary fiber, modified starch, and hydroxypropyl methylcellulose (HPMC) were prepared. A solution was prepared by dissolving maltodextrin into water to be 30 Bx concentration, and a solution was prepared by dissolving indigestible maltodextrin as a natural water-soluble dietary fiber into water to be 30 Bx concentration, and a solution was prepared by dissolving alpha-starch as a modified starch into water to be 10% concentration, and a solution was prepared by dissolving HPMC into a fermentation alcohol having a purity of 95% to be 5% by weight concentration.
[0094] 50 g of each psicose powder prepared in Preparative Example 1-3 and sugar, caster sugar, in which the average particle size was 230 m, were mixed to be the weight ratio of 1:1. After adding the prepared binding agent solution to the mixture, particles in the powder form were bound by passing through a 20 mesh sieve. In this state, after hot air drying at 45 C. for 30 to 50 minutes, granules were sieved evenly and collected. As the prepared binding agent solution, maltodextrin, indigestible maltodextrin and HPMC were added so that the final content of the binding agent in the total weight of granules was 1% by weight, and alpha-starch was added so that the final content of the binding agent in the total weight of granules was 0.2% by weight.
TEST EXAMPLE 1
Analysis of Particle Size of Powder
[0095] Particle size analysis equipment (equipment name Mastersizer 2000, manufacturer Malvern) is to measure the size of particle using laser diffraction technology, and it is analyzed in the manner of calculating the particle size by measuring the intensity of light scattered when the laser beam passes the dispersed fine particle sample. The particle size of each mixed ingredient was measure using the equipment, and the result was disclosed in the following Table 2.
TABLE-US-00002 TABLE 2 Average Ratio of average Particle particle particle size size size (compared with distribution Saccharides (m) psicose) (m) Psicose crystal 237 1.0 74-428 (standard) Sugar 684 2.9 336-1125 (granulated white sugar) Sugar (finely- 392 1.7 235-580 granulated sugar) Sugar (ultra-finely 230 0.9 126-356 granulated sugar) Sugar 72 0.3 9-142 (powdered sugar) Glucose (anhydrous) 295 1.2 75-530 Glucose 261 1.1 79-512 (hydrated)
TEST EXAMPLE 2
Analysis of Mixing Level of Mixed Granule
[0096] The sugar composition of each sample was confirmed by partially collecting granules of three portions of top, middle and bottom, and analyzing by high performance liquid chromatography, after placing the granular powder prepared in Example 1-5 in a bag and vibrating for 10 minutes in a vibrator. The result was shown in Table 3 and Table 4. It was determined that the granular sugar was uniformly mixed well to a level that the deviation of sugar composition was 1% or less between mixed ingredients in the granular powder.
TABLE-US-00003 TABLE 3 Sugar composition (%) Example 1-1 Example 1-2 Psicose 49.1 50.7 Glucose 50.9 49.3 Sugar composition 0.4 0.2 deviation Mixing level (Mixing level: very high -, high-, low- (X))
[0097] As shown in Table 3, it was confirmed that a granular powder particle having less compositional deviation and uniform composition could be prepared than the simply mixing method, as granules were well formed by the binding solution, since the average particle size ratio of the two ingredients to be mixed was psicose:glucose=1.0:1.1 to 1.2 (refer to Table 2) in Example 1, and the particle size between the two ingredients was similar.
TABLE-US-00004 TABLE 4 Ingredient composition Example 2 Example 3 (wt %) 2-1 2-2 2-3 2-4 3-1 3-2 3-3 3-4 Psicose 50.9 49.3 51.0 40.1 51.4 50.2 51.0 50.6 Sugar 49.1 50.7 49.0 59.9 47.8 49.6 48.8 48.9 Binding agent 0.8 0.2 0.2 0.5 Sugar 0.9 0.3 1.0 4.3 0.8 0.1 0.5 0.4 composition deviation Mixing level X (Mixing level: very high, high, low(X))
[0098] In Example 2-4, it was difficult to prepare the mixed granular powder with uniform composition even when using a binding solution, since the average particle size of sugar was more than 4 times larger than psicose. However, except Example 2-4, it was confirmed that a granular powder with less compositional deviation and uniform composition could be prepared in the mixed granular powder (Example 2-1, 2-2, 2-3), which is within the range of psicose:sugar=1.0:0.31.7.
[0099] In addition, as a result of preparing a mixed granule of psicose and sugar according to the kinds of binding solutions in Example 3, it was confirmed that a granular powder with uniform composition could be prepared, since mostly a granule was well formed, although there was a slight difference according to the kinds of binding solutions.
TEST EXAMPLE 3
Sensory Evaluation of Psicose Mixed Granular Powder
[0100] Granular powder samples for sensory evaluation of the mixed saccharide granules of psicose and sugar were prepared by a simple granulation method using a binding solution as a fermentation alcohol. The powder of psicose of Example 1-3 was mixed with sugar, caster sugar to be a ratio of 9:1, 7:3, 5:5 (w/w) respectively. After adding a fermentation alcohol with a purity of 95% to 510% of the weight by mixing 100 g each, particles in the powder form were bound each other by passing through a 20 mesh sieve. In this state, after hot air drying at 45 C. for 30 to 60 minutes, granules were sieved evenly and collected. The collected mixed saccharide was named SP91, SP73 and SP55 according to the ratio of 9:1, 7:3, 5:5 (w/w), according to the mixing ratio of psicose powder and sugar.
[0101] Granular powder samples for sensory evaluation of the mixed saccharide granules of psicose and glucose were prepared by a simple granulation method using a binding solution as a fermentation alcohol. The powder of psicose of Example 1 was mixed with anhydrous glucose to be a ratio of 7:3, 5:5 3:7 (w/w) respectively. After adding a fermentation alcohol with a purity of 95% to 510% of the weight by mixing 100 g each, particles in the powder form were bound each other by passing through a 20 mesh sieve. In this state, after hot air drying at 45 C. for 30 to 60 minutes, granules were sieved evenly and collected. The collected mixed saccharide was named GP73, GP55 and GP37 according to the ratio of 7:3, 5:5, 3:7 (w/w), according to the mixing ratio of psicose powder and anhydrous glucose.
[0102] Sensory evaluation of granular powder samples in which sugar or glucose was mixed with psicose was performed. Each sample was provided by collecting 0.7 g each and it was represented by three digit number randomly extracted using a random number table. The order of providing samples was always randomly decided and lukewarm water for rinsing mouth was provided together to test personnel. The sensory test room maintained a constant temperature (251 C.) and no odor.
[0103] 15 panelists who had a high level of understanding of sensory evaluation and had experience in sensory test were selected as the sensory test personnel. Training was conducted three times a week for 1 month, and took an average of 30 minutes per training session. As the content and method of evaluation, sensory properties of psicose mixed saccharide were evaluated as sweet taste, sour taste, bitter taste, refreshing sensation and continuity of sweet taste, and 15 cm line scale was used.
[0104] The values of the sensory evaluation result were shown in the following Tables 5 and 6, and the graph of sweetness profile of the sensory evaluation result was shown in
TABLE-US-00005 TABLE 5 Continuity Sweet Bad Sour Bitter Refreshing of sweet taste taste taste taste sensation taste Sugar 10.0 1.5 1.5 1.5 5.0 5.0 Psicose 7.3 6.0 4.2 5.1 10.0 8.2 SP91 9.8 5.1 2.7 3.6 4.5 9.5 SP73 9.2 5.4 3.0 3.8 6.5 8.7 SP55 8.3 5.6 3.0 4.4 8.9 8.6
TABLE-US-00006 TABLE 6 Continuity Sweet Bad Sour Bitter Refreshing of sweet taste taste taste taste sensation taste Glucose 8.6 5.3 3.4 3.3 4.1 7.3 Psicose 7.3 6.0 4.2 5.1 10.0 8.2 GP73 9.4 4.9 3.3 4.0 5.3 9.0 GP55 8.8 5.1 4.0 4.3 7.0 8.3 GP37 7.8 5.0 3.8 4.6 8.2 8.6
[0105] Improvement of sweetness quality is needed, since psicose has sweetness equivalent to 70% of sugar, but it has late sweetness increase or bitter taste or bad taste at the tail. Therefore, by mixing sugar or glucose at a certain ratio, a sweetener with improved taste can be provided by overcoming disadvantages of sweetness quality of psicose. As shown in the table of result of sensory evaluation, it was demonstrated that sweet taste was increased than psicose alone, and bad taste and bitter taste were alleviated, and particularly continuity of sweet taste was significantly increased than the conventional sugar, due to mixing of psicose and sugar. In addition, it was confirmed that sweet taste seemed to be stronger than psicose and glucose alone, respectively, and bad taste and bitter taste were alleviated to the level similar to the conventional glucose than psicose alone, because of mixing psicose and glucose. Especially, it was confirmed that continuity of sweet taste was significantly increased than the conventional sugar and glucose. It was judged that sweet taste was continued long and sweet taste was also felt strongly, because the refreshing sensation was magnified immediately upon ingestion, thereby complementing unique bad taste and bitter taste of psicose, and the late increase of sweetness caused synergy with sweet taste of sugar or glucose.
TEST EXAMPLE 4
Physical Properties of Psicose Mixed Saccharide Granule
[0106] (1) Evaluation of Flowability
[0107] 20 g of the sample was precisely weighed and placed in a funnel for measurement (Orifice 1.55 mm), and the time (second) in which all 20 g of the sample flowed down on the weighing scale, and the result was shown in the following Table 7 and
TABLE-US-00007 TABLE 7 Average value of flowability Deviation Percentage Sample (g/sec) (g/sec) (%) Psicose 3.78 0.37 100.0 Example 1-1 5.81 0.23 153.8 Example 1-2 4.54 0.19 120.1 Example 2-2 5.97 0.15 158.1 Example 2-3 5.72 0.21 151.5
[0108] It was confirmed that the flowability of the mixed granular powder with respect to the single psicose powder was improved to the level of 120 to 159% or more than psicose. As the flowability was improved, a company shipping particular or powdery products could be offered many benefits in the packaging and distribution steps.
[0109] (2) Evaluation of Hygroscopicity
[0110] 3 g of each sample was placed in a dish and stored in a thermohygrostat at a temperature of 40 C. and a relative humidity of 603% for 150 minutes, and the weight of each sample was measured after 50 min, 70 min and 150 min, and the result was shown in
TABLE-US-00008 TABLE 8 Hygroscopicity Percentage Sample increment (g) Percentage (%) deviation (%) Psicose 0.3356 100.0 Example 1-1 0.2850 85.2 1.26 Example 1-2 0.2580 77.0 3.56 Example 2-2 0.2952 88.2 5.47 Example 2-3 0.2011 60.4 10.09
[0111] As a result of comparing hygroscopicity of each sample in the graph of hygroscopicity increment of
TEST EXAMPLE 5
Differential Scanning Calorimeter (DSC) Analysis of Mixed Saccharide Granule and Composed Sugar Powder
[0112] In order to confirm that the prepared mixed saccharide granule was the mixed granule of the sugar powder in which chemical properties of the constitutional sugar powder of the mixed saccharide were maintained intact, differential scanning calorimeter (DSC) analysis method that can determine physical and chemical properties of samples from temperature and calorie change data (peak position, shape, number, area, etc.), which were obtained from energy provided into the assay samples of the mixed saccharide granule prepared in Example 1-1 and Example 2-2 and single material of each constitutional ingredient which composes that, was performed. The sample used for DSC measurement was as follows.
TABLE-US-00009 TABLE 9 Assay sample Detailed description Psicose powder Preparative Example 1-3 Glucose powder Anhydrous glucose powder with 295 m of the average particle size, used for preparation of the mixed saccharide granule of Example 1-1 Sugar powder ultra-finely granulated sugar with 230 m of the average particle size, used for preparation of the mixed saccharide granule of Example 2-2 Mixed saccharide granule Mixed saccharide granule of psicose and glucose obtained in Example 1-1 Mixed saccharide granule Mixed saccharide granule of psicose and sugar obtained in Example 2-2
[0113] The following DSC (differential scanning calorimeter) equipment and analysis information were used, and the result was shown in Table 10.
[0114] Equipment name: DSC [differential scanning calorimeter]
[0115] Manufacturer: Perkin Elmer
[0116] Model name: Diamond DSC
[0117] Analysis conditions: room temperature (RT) to 250 C. 10 C./min temperature rising, N2 gas purge, (standard method: refer to USA standard test method ASTM D 3418.)
TABLE-US-00010 TABLE 10 Endothermic peak Assay sample temperature(Tg, C.) Psicose powder 109.0 Glucose powder 162.2 Sugar powder 192.2 Mixed saccharide granule of Psicose: 109.4 psicose and glucose (Example 1-1) Glucose: 159.4 Mixed saccharide granule of Psicose: 109.4 psicose and sugar (Example 2-2) Sugar: 159.4
[0118] As shown in Table 10, it was demonstrated that distinct endothermic peaks of two mixed ingredients were detected in case of the mixed saccharide granules of the present invention. That is, the result of analyzing the sugar powder which is comprised in the mixed saccharide granule of the present invention alone and the result of constitutional ingredient which is comprised in the mixed saccharide all exhibited the same endothermic peak temperature, and this means that physical/chemical properties of each constitutional ingredient were maintained intact in the mixed saccharide granule.