CS211585B1 - Method of chromatographic separation of alditoles - Google Patents

Description

The invention relates to the chromatographic separation of alditols on a cation exchange column in a lanthanum cycle using water as the eluent.

Virtually all alditol mixtures are based on chromatographic methods. Borate ions utilize paper chromatography as a component of the chromatography system. R. Barker, D. C. C. Sraith, Chem. and Ind, 1954-19; Stankovic, V. Bilik, M. Kedoroňko,

J. Kanigstein, Chem. Announcement 29, 685 (9Ί5ί)> chromatography eluting with borate buffers on anion exchange columns in borate cycle / A. B. Foster, Adv. Varbohyd. Chem.12, 1114/1957, and activated carbon and jaw / S. A. Barker, E. J. Bouřné, 0. Theander, J. Chem. Soc. 195 5, 4276.7. The vapor distribution of some alditols was achieved on Fuller soil and cellulose / V columns. W. Binkley, Adv. Carbohyd. Chem. 10, 67 (1955), on the anion exchange in the sulphate cycle. Samuelson, H. Strb * mberg, Carbohyd. Res. 3, 89 (1966) and on cation exchangers in the lithium, calcium and barium cycles (J). Κ. N. Jones, R.A. Wall, Canad. J. Chem. 38, 2290 (1960): 0. Samuelson, H. Str Smberg, Acta Chem. Scand. 2, 1,252 (1,968); Angyal, S.J. Bethell, G., Beveridge, R.J., Carnohyd. Res. 73, 9 (1979); A.J. Melája, L. Hamalaineh, Ger. No. 2,418,801, C.A. 82, 73,397 (1975); A.J. Melaja, L. Hamalainen, L. Rantanen, U. S. 3,928,193, C.A. 8 5, 35,131 (1,976). The proposed mode of separation is very simple in conversion and allows efficient alditol separation, even such / e.g. galactitol - glucitol ,. mannitol - altritol /, which may be separated on cation exchangers cycled by alkali metal and alkaline earth metal cations.

The principle of the chromatographic separation of alditols according to the invention is that the mixture of alditols is chromatographed by elution with water on a column of cation exchange resin in a lanthanite cycle.

The advantage of the suggested methods of chromatographic separation are alditols, _x that enables quick and effective distribution of the mixture tetritolov, pentitols, hexitols, heptitolov, optionally a mixture of alditols rSznym number of carbon atoms in the molecule, allows to 5- to 15 weight% preload chromatographed e pic náplně'zmesou aldi.toiov (calculated on an air-dry ion exchanger), elution with water removes technical difficulties in using, resp. by finally removing the buffer solutions and organic solvents as elution systems; · Alditols of high purity are obtained,.

^{The κ} / chromatographic cartridge can be reused without regeneration and without decreasing the separation efficiency to virtually any number of separations.

Example l

The mixture .alpha./alitol, D-mannitol, D-altritol, galactitol, D-glucitol, L-iditol), respectively. mixture B (ribitol, L-arabinitol, xylitol, pentaerythritol, galactitol), mixture, C (erythritol, D-threitol, D-glucitol, D-glycero-D-taloheptitol, D-glycero-D-galactoheptitol), mixture D / glycerol,

D-threitol, D-xylitol, galactitol, D-glycero-D-taloheptitol (each alditol 0,1 0.1 g) are chromatographed at room temperature in a column (90 x 0.9 cm) with Dowex 50 W ion exchanger,

200-400 mesh in the La-cycle, eluting with water at a flow rate of 15 ml.h. The relative elution volumes V _{r of} each alditol relative to the elution volume of pentaerythritol V »54 ml, V _r = 1.00, are given in Table 1.

Relative elution volumes of alditols when chromatographed on Dowex 50 W in La-cycle eluting with water

alditol IN r glycerol • 0.99 erythritol 0.97 D-threitol 1.48 ribitol / adonit / 0.89 L-arabinitol. 1, 39 D-xylitol 2.52 allitol 0.91 D-mannitol 1.20 D-altritol 1, 35 galactitol / dulcite / 1.98 D-glucitol (eorbit) '2.50 L-iditol 3.15 D-glycero-D-taloheptitol / volemite / 1.17 D-glycero-D-galactoheptitol 1.70 pentaerythritol 1, 00

Example

The mixture (4 g) of D- [2- ² h] mannitol and D- [2- ^ 1] glucitol (obtained by reduction of D-fructose with sodium borate deutetide, after deionization with cation exchange resin, concentration and evaporation of the distillation residue with methanol three times) is chromatographed on The cation exchange column in the La-cycle shown in Example 1, eluting with water at a flow rate of 18 ml.h, separates unreacted from each other. the starting D-fructose / 0.1 g, elution volume 34-36 ml / ^, D- [2- ² H] mannitol / 1.9 g, 54-88 ml / ^1, and D [2 H ^2] glucitol (1.9 g, 100 to 16 * 5 ml).

Example 3

The mixture (0.8 g) of [3- [mu]] ribitol and xylitol (obtained by reduction of erythro-3-pentulose by boron sodium deuteride) is chromatographed on a cation exchange column in the La-cycle shown in Example 1, eluting with water at a flow rate of 40 ml / h. C ^{3 -2} Hj ribitol (0.4 g, elution volume 40-60 ml) and [3-h] xylitol (0.4 g 110-155 ml) were obtained.

Said method of chromatographic separation of alditols on the cation exchanger in the lanthanite cycle allows a simple and highly efficient separation of complex alditol mixtures which are of interest to the food industry and isotopically significant for monitoring chemical and biochemical reactions. At the same time, this method can be used in the preparative preparation of some rare alditols and in the analytical chemistry of carbohydrates.

Claims (1)

Method for chromatographic separation of alditols, characterized in that the mixture of alditols is chromatographed by elution with water on a column of a cation exchange resin in a lanthanite cycle.