MilliporeSigma
  • Home
  • Search Results
  • High efficiency, narrow particle size distribution, sub-2 μm based macrocyclic glycopeptide chiral stationary phases in HPLC and SFC.

High efficiency, narrow particle size distribution, sub-2 μm based macrocyclic glycopeptide chiral stationary phases in HPLC and SFC.

Analytica chimica acta (2015-11-04)
Chandan L Barhate, M Farooq Wahab, Zachary S Breitbach, David S Bell, Daniel W Armstrong
ABSTRACT

State of the art chiral chromatography still employs 3-5 μm bonded or immobilized chiral selectors in 10-25 cm columns. With the availability of 1.9 μm narrow particle size distribution (NPSD) silica, it is now possible to make ever shorter, high efficiency columns practical for sub-minute chiral separations. Three macrocyclic glycopeptides (teicoplanin, teicoplanin aglycone, and vancomycin) were bonded onto 1.9 μm NPSD particles. Such packed columns had ∼80% lower backpressure as compared to polydisperse (PD) 1.7 μm silica materials when using the same mobile phase. The decreased backpressure allowed for diminution of frictional heating and allowed for the use of the 1.9 μm NPSD particle based columns at high flow rates. The 1.9 μm NPSD particle based columns showed up to 190,000 plates m(-1) for chiral molecules and 210,000 plates m(-1) for achiral probes. Representative enantiomeric separations are shown for wide classes of compounds, including different types of amino acids, β-blockers, and pharmaceutically important heterocyclic compounds such as oxazolidinones. Applications in three liquid chromatography modes, namely, reversed phase, polar organic mode and normal phase chiral separations were shown with resolution values ranging from 1.5 to 5.7. Additionally, the same columns were used with supercritical fluid chromatography (SFC) for ultrafast separations.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
5α-Androstan-17β-ol-3-one, ≥97.5%
Sigma-Aldrich
Acetonitrile, ≥99.5%, ACS reagent
Sigma-Aldrich
Acetonitrile, anhydrous, 99.8%
Sigma-Aldrich
Toluene, anhydrous, 99.8%
Sigma-Aldrich
Pyridine, anhydrous, 99.8%
Sigma-Aldrich
Ethyl alcohol, Pure, 190 proof, ACS spectrophotometric grade, 95.0%
Sigma-Aldrich
Pyridine, ≥99%
Sigma-Aldrich
Ethyl alcohol, Pure, 190 proof, meets USP testing specifications
Sigma-Aldrich
3-(Triethoxysilyl)propyl isocyanate, 95%
Sigma-Aldrich
Ethyl alcohol, Pure, 200 proof, anhydrous, ≥99.5%
Supelco
Acetonitrile, HPLC grade, ≥99.93%
Sigma-Aldrich
Sodium hydrosulfite, ≥82% (RT)
Sigma-Aldrich
1,3-Dinitrobenzene, 97% anhydrous basis
Sigma-Aldrich
Hydrogen chloride, ReagentPlus®, ≥99%
Supelco
Methanol solution, NMR reference standard, 4% in methanol-d4 (99.8 atom % D), NMR tube size 5 mm × 8 in.
Sigma-Aldrich
Methanol solution, NMR reference standard, 4% in methanol-d4 (99.8 atom % D), NMR tube size 3 mm × 8 in.
Sigma-Aldrich
Acetonitrile, HPLC Plus, ≥99.9%, poly-coated bottles
Supelco
Toluene, HPLC grade, 99.8%
Sigma-Aldrich
Methanol-12C, 99.95 atom % 12C
Sigma-Aldrich
Toluene, suitable for HPLC, ≥99.9%
Supelco
Methanol solution, contains 0.10 % (v/v) formic acid, UHPLC, suitable for mass spectrometry (MS), ≥99.5%
Sigma-Aldrich
Ethanol, ACS reagent, prima fine spirit, without additive, F15 o1
Sigma-Aldrich
Trifluoroacetic acid, ReagentPlus®, 99%
Sigma-Aldrich
Acetonitrile
Sigma-Aldrich
Toluene, ACS reagent, ≥99.5%
Sigma-Aldrich
Acetonitrile, ReagentPlus®, 99%
Sigma-Aldrich
Pyridine, ReagentPlus®, ≥99%
Sigma-Aldrich
Trifluoroacetic acid, ≥99%, for protein sequencing
Sigma-Aldrich
Toluene, ACS reagent, ≥99.5%
Sigma-Aldrich
Pyridine, ReagentPlus®, ≥99%