Classifications

• • C—CHEMISTRY; METALLURGY
  • C13—SUGAR INDUSTRY
  • C13K—SACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
  • C13K1/00—Glucose; Glucose-containing syrups
  • C13K1/06—Glucose; Glucose-containing syrups obtained by saccharification of starch or raw materials containing starch

Definitions

• the present invention relates to a new process for preparing enzymatically converted glucose syrups which can be used as countertypes for standard acid converted glucose syrups, i.e. glucose syrups with a DE varying between 30 and 50, and to the new syrups which can be thus obtained.
• the acid process is generally used for syrups in the range of 30-50 DE (Dextrose Equivalent) .
• the acid conversion always yields a product of specific composition because of the random hydrolysis of the starch.
• Major disadvantages of this process are the high salt content of the syrup, and the special equipment needed to perform the acid conversion reaction.
• the acid converted glucose syrups are typically used in hard boiled candy. There they reduce the tendency of sucrose to crystallise, they slow down the tendency to shell-graining and they contribute to the body and "mouth- feel" of the confection on consumption. Glusose syrups are also used in toffees, fudge or fondant where they prevent, slow down or control granulation of sucrose. These acid converted glucose syrups represent a market of more than 400.000 ton dry substance Europe-wide.
• the glucose syrups according to the invention consist of a starch based, enzymatically converted glucose syrups, having a DE value (Dextrose Equivalent) between 30 and 50 and a sugar spectrum in which the fraction of DPI - DP3 ranges from 30 to 60 %, the fraction of DP4 - DP6 ranges from 25 to 16 %, the fraction of DP7 - DP9 ranges from 14 to 4 %, and the fraction above DP9 ranges from 38 to 18 %, on d.s. (dry substance).
• DE value Dextrose Equivalent
• Preferred glucose syrups according to the invention have a DE value between 36 and 45 and a sugar spectrum in which the fraction of DPI - DP3 ranges from 38 to 55 %, the fraction of DP4 - DP6 ranges from 24 to 17 %, the fraction of DP7 - DP9 ranges from 13 to 4,5 %, and the fraction above DP9 ranges from 32 to 21 %, on d. s.
• glucose syrups according to the invention have a DE value between 38 and 42 and by a sugar spectrum in which the fraction of DPI - DP3 ranges from 40 to 52 %, the fraction of DP4 - DP6 ranges from 24 to 18 %, the fraction of DP7 - DP9 ranges from 13 to 5 %, and the fraction above DP9 ranges from 30 to 22 %, on d.s..
• Applicants have also developped well determined conditions of a double enzymatic process allowing the preparation of such new glucose syrups. It is therefore also an object of the present invention to provide a new process for preparing glucose syrup by treating starch with enzymes.
• the process according to the invention comprises treating a liquified starch substrate by means of an enzyme mixture in a single enzymatic conversion step, whereas said enzyme mixture comprises a bacterial alpha amylase, a maltogenic amylase and a glucoamylase.
• the starting substrate for the process according to the invention is a liquified starch, as may for instance be obtained by liquifaction of native starch with a thermostable alpha amylase to a DE of 10-12, deactivation of the thermostable alpha amylase, and cooling of the liquified starch to a temperature of about 60°C.
• the enzymes used in the enzyme mixture according to the invention are widely available on the market.
• the preferred glucoamylase, exo-l,4-aplha-D- glucosidase can in particular be obtained from a selected strain of Aspergillus niger by submerged fermentation.
• the bacterial alpha amylase is preferably an endo-amylase which hydrolyses 1,4-alpha-glucosidic bonds in gelatinised starch.
• the alpha amylase can be produced by fermentation of a selected strain of Bacillus subtilis.
• the preferred maltogenic amylase (EC3.2.1.133) hydrolyses 1,4-alpha-glucosidic linkages in starch, partially hydrolysed starch and low-molecular weight oligosaccharides, including maltotriose. Maltose units are removed in a stepwise manner from the non-reducing chain ends.
• the enzyme which can come from Bacillus stearothermophilus, can be expressed in and produced by a genetically modified strain of Bacillus subtilis. For industrial applications the recommended operating conditions are 60°C and pH 5,0-5,5.
• the single enzymatic conversion step - i.e. a saccharification step - applied to the starting substrate in accordance with the invention is preferably performed at a temperature in the range from 55 to 65° C for a period of 10 to 48 hours, at a pH between 4,9 and 5,1; most preferably at a temperature in the range from 60 to 62° C for a period of 18 to 24 hours, at a pH between 4,9 and 5,1.
• the dry substance content of reaction mixture is preferably between 30 and 40% , more preferably between 32 and 37% , and most preferably between 33 and 35% .
• the process according to the invention is particularly suitable for preparing the new glucose syrups according to the invention as defined above.
• the enzyme concentrations and the enzyme ratios during the enzymatic conversion step according to the invention entirely depend on the process conditions applied and on the specific properties of the glucose one wishes to obtain.
• concentrations will readily be determined by the skilled art worker on the basis of the data provided by the supplier of the commercial enzymes used in the process and/or by using mathematical calculations on the basis of empirical models, as is already known in the art (report A-05944a-GB by NOVO : "Development and field confirmation of a mathematival model for amyloglucosidase/pullulanase saccharification" by T.R. Swanson et al.
• An empirical model can be construed based on information obtained from a design set-up of experiments of saccharification tests. By selecting an appropriate model, equations are obtained by which the amount (%w/w) of the different DP fractions in function of the concentrations of the different enzymes and the time can be calculated.
• Native starch was suspended in water at a concentration of 33-35% d.s. and at a slightly acidic pH
• thermostable alpha amylase was added (0,5-0, 6ml comm./kg d.s.). This slurry was then further liquified during 2-3 hours at 90-95°C until a DE of 10-12 was reached. Then the alpha amylase was inactivated by adjusting the pH to 4 while heating the liquefied starch for an additional 5 minutes at 95°C.
• This substrate was then cooled to 60°C and pH was adjusted to 5,0.
• a mixture of enzymes was added composed of a glucoamylase, a maltogenic amylase and a bacterial alpha amylase. The following enzyme quantities were used :
• an enzymatically converted 38DE syrup was obtained having a composition and properties comparable to those of an acid converted 38DE syrup, (cf table 2) :
• Example 2 (2) viscosity at 80% d.s. and 50°C
• Native starch was suspended in water at a concentration of 33-35% d.s. and at a slightly acidic pH (3,5-4,0). This slurry was then gelatinised at 160°C. After cooling to 95°C, pH was adjusted to 5,7-5,9 and thermostable alpha amylase was added (0,5-0, 6ml comm/kg d.s.). This slurry was then further liquified during 2-3 hours at 90-95°C until a DE of 10-12 is reached. Then the alpha amylase was inactivated by adjusting the pH to 4 while heating the liquified starch for an additional 5 minutes at 95°C.
• This substrate was then cooled to 60°C and pH is adjusted to 5,0.
• a mixture of enzymes was added composed of a glucoamylase, a maltogenic amylase and a bacterial alpha amylase. The following enzyme quantities were added : - .AMG 300 L : 16,5 AGU/kg d.s. - maltogenase 4000L : 48 MANU/kg d.s.

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• Chemical & Material Sciences (AREA)
• Health & Medical Sciences (AREA)
• Emergency Medicine (AREA)
• General Health & Medical Sciences (AREA)
• Life Sciences & Earth Sciences (AREA)
• Biochemistry (AREA)
• Organic Chemistry (AREA)
• Jellies, Jams, And Syrups (AREA)
• Preparation Of Compounds By Using Micro-Organisms (AREA)
• Saccharide Compounds (AREA)

Priority Applications (7)

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Citations (2)

• 1996
  • 1996-09-17 ES ES96931816T patent/ES2169263T3/es not_active Expired - Lifetime
  • 1996-09-17 AU AU70857/96A patent/AU7085796A/en not_active Withdrawn
  • 1996-09-17 WO PCT/EP1996/004088 patent/WO1998012342A1/en active IP Right Grant
  • 1996-09-17 DE DE69618025T patent/DE69618025T2/de not_active Expired - Fee Related
  • 1996-09-17 AT AT96931816T patent/ATE210730T1/de not_active IP Right Cessation
  • 1996-09-17 EP EP96931816A patent/EP0929690B1/de not_active Expired - Lifetime
• 1999
  • 1999-03-16 BG BG103254A patent/BG64008B1/bg unknown

Patent Citations (2)

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