US3694158A - Process for the simultaneous determination of glucose and fructose - Google Patents

Process for the simultaneous determination of glucose and fructose Download PDF

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Publication number
US3694158A
US3694158A US14706A US3694158DA US3694158A US 3694158 A US3694158 A US 3694158A US 14706 A US14706 A US 14706A US 3694158D A US3694158D A US 3694158DA US 3694158 A US3694158 A US 3694158A
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United States
Prior art keywords
fructose
glucose
solutions
simultaneous determination
refractive index
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Expired - Lifetime
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US14706A
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English (en)
Inventor
Karl Lauer
Helmut Spingler
Karl-Erhard Wallach
Georg Stoeck
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Cf Boehringer & Soehne GmbH
Roche Diagnostics GmbH
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Boehringer Mannheim GmbH
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/41Refractivity; Phase-affecting properties, e.g. optical path length
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/21Polarisation-affecting properties
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/02Food
    • G01N33/14Beverages
    • G01N33/143Beverages containing sugar
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10TTECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T436/00Chemistry: analytical and immunological testing
    • Y10T436/14Heterocyclic carbon compound [i.e., O, S, N, Se, Te, as only ring hetero atom]
    • Y10T436/142222Hetero-O [e.g., ascorbic acid, etc.]
    • Y10T436/143333Saccharide [e.g., DNA, etc.]
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10TTECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T436/00Chemistry: analytical and immunological testing
    • Y10T436/14Heterocyclic carbon compound [i.e., O, S, N, Se, Te, as only ring hetero atom]
    • Y10T436/142222Hetero-O [e.g., ascorbic acid, etc.]
    • Y10T436/143333Saccharide [e.g., DNA, etc.]
    • Y10T436/144444Glucose

Definitions

  • I50 A I a U1 GRAMS PER LITER 0 30 6O 90 :20 I50 I80 m [ ⁇ VEYTORS l6 LITERS PER HOUR KAF-eL L-AUER HELMUT SPINGLER B Y KARL-ERHARD WALLACF GEORG ST ECK Sept. 26, 1972 K. LAUER ETAL 3,694,158
  • the present invention is concerned with a process for the simultaneous determination of glucose and fructose, and more particularly with the simultaneous determination, without delay, in warm (50 to 75 C.), aqueous solutions.
  • the process of the type provided by the present invention is an essential requirement for being able to carry out, on a large scale, the separation of glucose and fructose on ion exchanger columns (c.f. US. Pat. No. 3,044,904 and US. patent application Ser. No. 569,362, filed Aug. 1, 1966, now abandoned. All previously used and known analytical procedures for the determination of glucose and fructose cannot be used for the abovementioned purpose because the determination of the two components in a continuously operating process is too complicated and, in particular, is too laborious.
  • an object of the invention to provide a simple, quick and continuous determination of glucose and fructose in eluates derived from ion exchange columns, in which an invert sugar solution has been separated into its components.
  • Another object of this invention is a process for the simultaneous determination of glucose and fructose in eluates derived from ion exchange columns, wherein the analytical data can be achieved in the form of proportional voltages.
  • a further object of this invention is a process for the determination of glucose and fructose which can be used for the automatic control of the flow of the eluates of ion exchange columns.
  • glucose and fructose can be determined simultaneously from warm aqueous solutions thereof when the angle of rotation (at) and the refractive index (n) of these solutions are measured and the concentrations of the components calculated therefrom in known manner.
  • the applicants herein have surprisingly found that this method of analysis can be relied on although the final optical rotation of glucose-fructose solutions is, upon cooling, only slowly adjusted (i.e. in 0.5-1 hour) (c.f.
  • glucose and fructose can be determined simultaneously and substantially without delay by means of the refractive index and angle of rotation when the measurement of these two physical proper ties is not carried out, as is usual, at 20 C. but at a temperature which is the same as or higher than the temperature of the original solution.
  • the adjustment of the optical rotation then takes place so quickly that the values obtained can even be used, via an automatic computer, for example, an analogue computer, for the automatic control of the separating column.
  • these continuously operating devices also permit the measurement results to be taken off simultaneously as proportional voltages which can be fed into an automatic computer, preferably a programcontrolled computer, the results of which can be used for controlling the whole plant, or can be supplied to multicolor recording apparatus, the results then being obtained in the form of a diagram.
  • FIG. 1 shows such a new nomogram for evaluating the amounts of fructose and glucose in a 60 C. warm aqueous solution by means of the angle of rotation and the refractive index at 60 C. being achieved by a series of calibration values at 60 C.;
  • FIG. 2 shows a diagram which was prepared from a series of single evaluations according to this invention by means of the nomogram, of the sugar content of the effluent of an ion exchange resin column separating fructose and glucose at 60 C., and
  • FIG. 3 shows a diagram which was prepared from an analogous series of single evaluations as in FIG. 2, the measurement however being done at 20 C. by prior cooling of the eflluent to 20 C. and using a 20 C. nomogram.
  • the fructose seems still to contain substantially high amounts of glucose, though as can be shown by checking this result by means of conventional analysis, the fructose fractions contain less or no glucose.
  • the process according to the present invention is, of course, not only suitable for the analysis of eluates of invert sugar solutions separated on ion exchangers (for example according to US. Pat. No. 3,044,904 and copending US. application Ser. No. 569,362 according to German patent application No. B 83,146 IVa/89i), but is, in principle, suitable for the analysis of all warm sugar solutions on a technically satisfactory scale.
  • EXAMPLE 1 Discontinuous, rapid determination of glucose and froctose in eluates from an ion exchanger column
  • EXAMPLE 2 For comparison, the sugar solution emerging from the column, before entering into the measuring devices, was passed through a cooler and thus cooled to exactly 20 C. The refractive index and optical rotation were read oif every 10 minutes and evaluated by means of a nomogram calculated for 20 C. The values for glucose and fructose were, in the manner described above, incorporated into a graph (see FIG. 3 of the accompanying drawings); this showed that the fructose was apparently still contaminated with considerable amounts of glucose. The re-examination of this result with previously used but time-consuming analytical procedures for the determination of fructose and glucose showed that false results had clearly been obtained which were due to the slow adjsutment to the final optical rotation of the fructose.
  • EXAMPLE 3 Measuring at higher temperatures than the temperatures of the eflluent of a chromatographic column
  • EXAMPLE 4 Continuous, rapid determination of glucose and fructose in eluates from an ion exchanger column A part of the eluate emerging at a temperature of 60 C. from the end of an ion exchanger column was passed, via the shortest possible polyethylene tube, through a continuously registering polarimeter (Zeiss) and through a continuously registering refractograph (Zeiss), from which the measurement values could also be taken off in the form of a proportional voltage. The current of liquid was subsequently again returned to the main current of the eluate.
  • Zeiss continuously registering polarimeter
  • Zeiss continuously registering refractograph
  • the measurement voltages of the polarimeter and of the refractograph were fed into an analogue computor (Zeiss) which gave the concentrations of glucose and fructose, with the help of a multi-color recording device, as a continuous elution diagram similar to that in FIG. 2.
  • valves were operated which directed into three separate containers the fractions which follow one another, i.e. glucose, glucose+fructose, fructose, fructose-l-glucose, glucose, etc.
  • the solutions in question were passed into a collecting vessel for mixed fractions which were mixed with fresh invert sugar and subsequently again passed through the separating column.
  • the fractions consisting of pure fructose solution and pure glucose solution were worked up separately in the conventional manner, for example by evaporation and crystallization.
  • Process for the continuous and simultaneous determination of glucose and fructose in an aqueous solution thereof having a temperature of about 50 to about 75 C. comprising measuring the optical rotation and refractive index of said solution by means of a continuously registering polarimeter and refractograph, and relating said measurements to the concentrations of both glucose and fructose in said solution.
  • Process for the continuous and simultaneous determination of glucose and fructose in an aqueous solution thereof having a temperature of about 50 to about 75 0. comprising measuring of the optical rotation and refractive index of said solution by means of a continuously registering polarimeter and refractograph, using the optical rotation and refractive index measurements, respectively, to calculate therefrom the concentrations of glucose and fructose, respectively in said solution by comparison of such measurements with measurements of a known sample or known samples.
  • Process according to claim 5 which comprises utilizing said signals in a data processing system which in turn is adapted to control the manufacture of said glucose and fructose in aqueous solution.

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  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Biochemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Pathology (AREA)
  • Physics & Mathematics (AREA)
  • Analytical Chemistry (AREA)
  • Immunology (AREA)
  • General Health & Medical Sciences (AREA)
  • Food Science & Technology (AREA)
  • Engineering & Computer Science (AREA)
  • Medicinal Chemistry (AREA)
  • Investigating Or Analysing Biological Materials (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)
  • Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
  • Saccharide Compounds (AREA)
US14706A 1965-12-15 1970-02-20 Process for the simultaneous determination of glucose and fructose Expired - Lifetime US3694158A (en)

Applications Claiming Priority (1)

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DEB0084982 1965-12-15

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US (1) US3694158A (en, 2012)
JP (1) JPS5313989B1 (en, 2012)
AT (1) AT273545B (en, 2012)
BE (1) BE818037Q (en, 2012)
CH (1) CH444527A (en, 2012)
DE (1) DE1598082B2 (en, 2012)
FI (1) FI48018C (en, 2012)
FR (1) FR1508973A (en, 2012)
GB (1) GB1095210A (en, 2012)
NL (1) NL152985B (en, 2012)
SE (1) SE323539B (en, 2012)

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3826905A (en) * 1971-10-27 1974-07-30 Suomen Sokeri Oy Methods and apparatus for providing automatic control of chromatographic fractionating processes
US4102646A (en) * 1977-04-06 1978-07-25 Sleeter Ronald T Quantitative analysis of carbohydrates by infrared spectroscopy
US4155774A (en) * 1977-08-09 1979-05-22 Randolph Ellwood A Process for controlling the rate of growth of particulate masses
US4182633A (en) * 1976-12-21 1980-01-08 Mitsubishi Chemical Industries Limited Process of the operation of a simulated moving bed
US4278438A (en) * 1978-04-20 1981-07-14 Willem Walraven Method and apparatus for analysis of saccharides
US6093326A (en) * 1993-01-26 2000-07-25 Danisco Finland Oy Method for the fractionation of molasses
US6214125B1 (en) 1994-09-30 2001-04-10 Danisco Finland Oy Fractionation method for sucrose-containing solutions
US6224776B1 (en) 1996-05-24 2001-05-01 Cultor Corporation Method for fractionating a solution
US6663780B2 (en) 1993-01-26 2003-12-16 Danisco Finland Oy Method for the fractionation of molasses
US6896811B2 (en) 2001-05-09 2005-05-24 Danisco Sweeteners Oy Chromatographic separation method

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3609324A (en) * 1968-02-10 1971-09-28 Zeiss Stiftung Method and apparatus for measuring the purity ratio of intermediate products in sugar manufacture
DE1962864C2 (de) * 1968-12-30 1982-09-09 Központi Elelmiszeripari Kutató Intézet, Budapest Verfahren zur Bestimmung der Zusammensetzung von Stoffgemischen bezüglich deren Bestandteile
US3724957A (en) * 1971-03-04 1973-04-03 Yokogawa Electric Works Ltd Concentration measuring apparatus
DE19545018A1 (de) * 1995-12-02 1997-06-05 Marcel Kastler Computergesteuertes Polarimeter zur Drehwinkelbeobachtung von Reaktionen unter konstanten Versuchsbedingungen
US8092609B2 (en) 2007-02-05 2012-01-10 European Sugar Holdings S.A.R.L. Sucrose inversion process

Cited By (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3826905A (en) * 1971-10-27 1974-07-30 Suomen Sokeri Oy Methods and apparatus for providing automatic control of chromatographic fractionating processes
US4182633A (en) * 1976-12-21 1980-01-08 Mitsubishi Chemical Industries Limited Process of the operation of a simulated moving bed
US4102646A (en) * 1977-04-06 1978-07-25 Sleeter Ronald T Quantitative analysis of carbohydrates by infrared spectroscopy
US4155774A (en) * 1977-08-09 1979-05-22 Randolph Ellwood A Process for controlling the rate of growth of particulate masses
US4278438A (en) * 1978-04-20 1981-07-14 Willem Walraven Method and apparatus for analysis of saccharides
US6663780B2 (en) 1993-01-26 2003-12-16 Danisco Finland Oy Method for the fractionation of molasses
US6187204B1 (en) 1993-01-26 2001-02-13 Danisco Finland Oy Method for the fractionation of molasses
US6649066B2 (en) 1993-01-26 2003-11-18 Danisco Finland Oy Method for the fractionation of molasses
US6093326A (en) * 1993-01-26 2000-07-25 Danisco Finland Oy Method for the fractionation of molasses
US6214125B1 (en) 1994-09-30 2001-04-10 Danisco Finland Oy Fractionation method for sucrose-containing solutions
US6482268B2 (en) 1994-09-30 2002-11-19 Danisco Finland Oy Fractionation method for sucrose-containing solutions
US6685781B2 (en) 1994-09-30 2004-02-03 Danisco Sweeteners Oy Fractionation method for sucrose-containing solutions
US6224776B1 (en) 1996-05-24 2001-05-01 Cultor Corporation Method for fractionating a solution
US6572775B2 (en) 1996-05-24 2003-06-03 Cultor Corporation Method for fractionating a solution
US6875349B2 (en) 1996-05-24 2005-04-05 Cultor Corporation Method for fractionating a solution
US6896811B2 (en) 2001-05-09 2005-05-24 Danisco Sweeteners Oy Chromatographic separation method
US7229558B2 (en) 2001-05-09 2007-06-12 Danisco Sweeteners Oy Chromatographic separation method

Also Published As

Publication number Publication date
DE1598082A1 (de) 1970-04-09
SE323539B (en, 2012) 1970-05-04
JPS5313989B1 (en, 2012) 1978-05-13
CH444527A (de) 1967-09-30
NL6610982A (en, 2012) 1967-06-16
AT273545B (de) 1969-08-11
FI48018C (fi) 1977-07-08
FI48018B (en, 2012) 1974-01-31
DE1598082B2 (de) 1972-04-06
BE818037Q (fr) 1975-01-24
FR1508973A (fr) 1968-01-12
GB1095210A (en) 1967-12-13
NL152985B (nl) 1977-04-15

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