Chiral separations by HPLC on immobilized polysaccharide chiral stationary phases.

Chiral separations by HPLC on immobilized polysaccharide chiral stationary phases.

Methods in molecular biology (Clifton, N.J.) (2013-01-04)

Imran Ali, Zeid A Al-Othman, Hassan Y Aboul-Enein

ZUSAMMENFASSUNG

Immobilized polysaccharide chiral stationary phases (CSPs) are a new development in chiral chromatography with increasing importance for the resolution of racemic compounds. These CSPs can be used with solvents traditionally applied for the classical coated polysaccharide CSPs as well as solvents that were "forbidden" for the coated phases such as tetrahydrofuran, chloroform, dichloromethane, acetone, 1,4-dioxane, ethylacetate, and certain ethers. However, these forbidden solvents may be required for the determination of the chiral recognition mechanism. Therefore, the immobilized CSPs are effective for the evaluation of chiral recognition mechanisms. Furthermore, immobilized chiral columns are also useful for monitoring the progress of stereospecific synthetic reactions which are normally performed in such solvents. The present chapter describes the detailed experimental protocol of a chiral resolution on immobilized polysaccharides CSPs by HPLC.

MATERIALIEN

Produktnummer

Marke

Produktbeschreibung

34865

Sigma-Aldrich

Tetrahydrofuran, inhibitor-free, suitable for HPLC, ≥99.9%

34856

Sigma-Aldrich

Dichlormethan, suitable for HPLC, ≥99.8%, contains amylene as stabilizer

D65100

Sigma-Aldrich

Dichlormethan, contains 40-150 ppm amylene as stabilizer, ACS reagent, ≥99.5%

650463

Sigma-Aldrich

Dichlormethan, HPLC Plus, for HPLC, GC, and residue analysis, ≥99.9%, contains 50-150 ppm amylene as stabilizer

360589

Sigma-Aldrich

Tetrahydrofuran, contains 200-400 ppm BHT as inhibitor, ACS reagent, ≥99.0%

401757

Sigma-Aldrich

Tetrahydrofuran, anhydrous, ≥99.9%, inhibitor-free

270997

Sigma-Aldrich

Dichlormethan, anhydrous, ≥99.8%, contains 40-150 ppm amylene as stabilizer

186562

Sigma-Aldrich

Tetrahydrofuran, anhydrous, contains 250 ppm BHT as inhibitor, ≥99.9%

360481

Sigma-Aldrich

1,4-Dioxan, ACS reagent, ≥99.0%, contains ≤25 ppm BHT as stabilizer

34857

Sigma-Aldrich

1,4-Dioxan, suitable for HPLC, ≥99.5%

676934

Sigma-Aldrich

1,4-Dioxan, ACS reagent, ≥99.0%, contains <=25 ppm BHT as stabilizer

320269

Sigma-Aldrich

Dichlormethan, ACS reagent, ≥99.5%, contains 40-150 ppm amylene as stabilizer

676764

Sigma-Aldrich

Tetrahydrofuran, ACS reagent, ≥99.0%, contains 200-400 ppm BHT as inhibitor

02575

Supelco

Dichlormethan, analytical standard

76887

Supelco

1,4-Dioxan, analytical standard

676853

Sigma-Aldrich

Dichlormethan, ACS reagent, ≥99.5%, contains 40-150 ppm amylene as stabilizer

CRM48367

Supelco

1,4-Dioxan-Lösung, certified reference material, 2000 μg/mL in methanol, ampule of 1 mL

270385

Supelco

Tetrahydrofuran, HPLC grade, ≥99.9%, inhibitor-free

78445

Supelco

Tetrahydrofuran, analytical standard

439223

Sigma-Aldrich

Dichlormethan, suitable for HPLC, ≥99.9%, contains 40-150 ppm amylene as stabilizer

494453

Sigma-Aldrich

Dichlormethan, biotech. grade, 99.9%, contains 40-150 ppm amylene as stabilizer

551368

Sigma-Aldrich

1,4-Dioxan -Lösung, suitable for NMR (reference standard), 40% in benzene-d₆ (99.6 atom % D)

87369

Supelco

Tetrahydrofuran, Selectophore^™, ≥99.5%

66742

Supelco

Dichlormethan, Selectophore^™, ≥99.5%

736171

Supelco

1,4-Dioxan -Lösung, suitable for NMR (reference standard), 40% in benzene-d₆ (99.6 atom % D), NMR tube size 5 mm × 8 in.

704814

Sigma-Aldrich

1,4-Dioxan -Lösung, suitable for NMR (reference standard), 10 mM in D₂O ("100%", 99.96 atom % D), NMR tube size 5 mm × 7 in.

684228

Sigma-Aldrich

1,4-Dioxan -Lösung, suitable for NMR (reference standard), 40% in benzene-d₆ (99.6 atom % D), NMR tube size 10 mm × 8 in.

612073

Sigma-Aldrich

1,4-Dioxan -Lösung, suitable for NMR (reference standard), 40% in benzene-d₆ (99.6 atom % D), chromium(III) acetylacetonate 5 mg/mL, NMR tube size 3 mm × 8 in.

611905

Sigma-Aldrich

1,4-Dioxan -Lösung, suitable for NMR (reference standard), 40% in benzene-d₆ (99.6 atom % D), chromium(III) acetylacetonate 5 mg/mL, NMR tube size 5 mm × 8 in.

631868

Supelco

1,4-Dioxan -Lösung, suitable for NMR (reference standard), 5 mM in chloroform-d (99.8 atom % D), NMR tube size 3 mm × 8 in.