Merck
  • Home
  • Search Results
  • Separation of derivatized glucoside anomers using supercritical fluid chromatography.

Separation of derivatized glucoside anomers using supercritical fluid chromatography.

Journal of chromatography. A (2015-09-29)
Fernando Montañés, Paul Rose, Stephen Tallon, Rahau Shirazi
ABSTRACT

Preparative scale supercritical fluid chromatography was used to separate derivatized anomeric monosaccharides. Methyl 2,3,4,6-tetra-O-benzoyl-α-d-glucopyranoside and methyl 2,3,4,6-tetra-O-benzoyl-β-d-glucopyranoside were synthesized by benzoyl derivatization of the parent anomerically pure monosaccharides. The elution profiles of each anomer were studied, suggesting that separation was possible. Mixtures of the compounds were then prepared at different ratios and separation was achieved using carbon dioxide/ethanol mixtures as the mobile phase and GreenSep™ 5micron particle size silica as the stationary phase. Ethanol co-solvent in the mobile phase was required to give a successful separation of the anomers however over the range 6.5-10.4wt% ethanol concentration studied here there was little variation in the degree of separation. In fractionation trials, separation of mixtures into fractions with >98% purity was achieved, with recoveries greater than 96%.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Acetone-d6, 99.9 atom % D, contains 0.03 % (v/v) TMS
Sigma-Aldrich
Chloroform, anhydrous, contains amylenes as stabilizer, ≥99%
Sigma-Aldrich
Acetone-d6, 99.9 atom % D
Sigma-Aldrich
Acetone-d6, 99.9 atom % D
Sigma-Aldrich
Acetone-d6, 99.9 atom % D, contains 1 % (v/v) TMS
Sigma-Aldrich
Acetone-d6, 99.9 atom % D
Sigma-Aldrich
Sodium sulfate, BioUltra, anhydrous, ≥99.0% (T)
Sigma-Aldrich
Acetone-d6, ≥99.9 atom % D, contains 0.03 % (v/v) TMS
Sigma-Aldrich
Sodium sulfate, BioXtra, ≥99.0%
Sigma-Aldrich
Sodium sulfate, ≥99.0%, suitable for plant cell culture
Sigma-Aldrich
Chloroform, ≥99%, PCR Reagent, contains amylenes as stabilizer
Sigma-Aldrich
Acetone-d6, 99.9 atom % D
Sigma-Aldrich
Acetone-d6, "100%", 99.96 atom % D
Sigma-Aldrich
Sodium sulfate, ≥99.99% trace metals basis
Sigma-Aldrich
Sodium sulfate, Vetec, reagent grade, 99%
Supelco
Ethanol solution, certified reference material, 2000 μg/mL in methanol
Sigma-Aldrich
Benzoyl chloride, ReagentPlus®, ≥99%
Sigma-Aldrich
Chloroform, anhydrous, ≥99%, contains 0.5-1.0% ethanol as stabilizer
Sigma-Aldrich
Benzoyl chloride, ACS reagent, 99%
Sigma-Aldrich
Sodium sulfate, anhydrous, free-flowing, Redi-Dri, ReagentPlus®, ≥99%
Sigma-Aldrich
Chloroform, contains ethanol as stabilizer, ACS reagent, ≥99.8%
Sigma-Aldrich
Sodium sulfate, puriss. p.a., ACS reagent, reag. ISO, reag. Ph. Eur., anhydrous, ≥99.0%
Sigma-Aldrich
Sodium sulfate, anhydrous, free-flowing, Redi-Dri, ACS reagent, ≥99%
Sigma-Aldrich
Sodium sulfate, ACS reagent, ≥99.0%, anhydrous, granular
Sigma-Aldrich
Chloroform, puriss. p.a., reag. ISO, reag. Ph. Eur., 99.0-99.4% (GC)
Sigma-Aldrich
Chloroform, contains 100-200 ppm amylenes as stabilizer, ≥99.5%
Sigma-Aldrich
Chloroform, ReagentPlus®, ≥99.8%, contains 0.5-1.0% ethanol as stabilizer
Sigma-Aldrich
Sodium sulfate, puriss., meets analytical specification of Ph. Eur., BP, USP, anhydrous, 99.0-100.5% (calc. to the dried substance)
Sigma-Aldrich
Sodium sulfate, ACS reagent, ≥99.0%, anhydrous, powder
Sigma-Aldrich
Chloroform, ACS spectrophotometric grade, ≥99.8%, contains 0.5-1.0% ethanol as stabilizer