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  • Evaluation of stationary phases packed with superficially porous particles for the analysis of pharmaceutical compounds using supercritical fluid chromatography.

Evaluation of stationary phases packed with superficially porous particles for the analysis of pharmaceutical compounds using supercritical fluid chromatography.

Journal of chromatography. A (2014-08-19)
Alexandre Grand-Guillaume Perrenoud, William P Farrell, Christine M Aurigemma, Nicole C Aurigemma, Szabolcs Fekete, Davy Guillarme
ABSTRACT

Superficially porous particles (SPP), or core shell particles, which consist of a non-porous silica core surrounded by a thin shell of porous silica, have gained popularity as a solid support for chromatography over the last decade. In the present study, five unbonded silica, one diol, and two ethylpyridine (2-ethyl and 4-ethyl) SPP columns were evaluated under SFC conditions using two mixtures, one with 17 drug-like compounds and the other one with 7 drug-like basic compounds. Three of the SPP phases, SunShell™ 2-ethylpyridine (2-EP), Poroshell™ HILIC, and Ascentis(®) Express HILIC, exhibited superior performances relative to the others (reduced theoretical plate height (hmin) values of 1.9-2.5 for neutral compounds). When accounting for both achievable plate count and permeability of the support using kinetic plot evaluation, the Cortecs™ HILIC 1.6μm and Ascentis(®) Express HILIC 2.7μm phases were found to be the best choices among tested SPPs to reach efficiencies up to 30,000 plates in the minimum amount of time. For desired efficiencies ranging from 30,000 to 60,000 plates, the SunShell™ 2-EP 2.6μm column clearly outperformed all other SPPs. With the addition of a mobile phase additive such as 10mM ammonium formate, which was required to elute the basic components with sharp peaks, the Poroshell™ HILIC, SunShell™ Diol and SunShell™ 2-EP phases represent the most orthogonal SPP columns with the highest peak capacities. This study demonstrates the obvious benefits of using columns packed with SPP on current SFC instrumentation.

MATERIALS
Product Number
Brand
Product Description

Supelco
Thymine(Zidovudine Related Compound C), Pharmaceutical Secondary Standard; Certified Reference Material
USP
Warfarin, United States Pharmacopeia (USP) Reference Standard
Sulfadimethoxine for peak identification, European Pharmacopoeia (EP) Reference Standard
Resorcinol, European Pharmacopoeia (EP) Reference Standard
Supelco
Ascentis® Express HILIC, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 3 cm × 3 mm
Supelco
Ascentis® Express HILIC, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 5 cm × 3 mm
Supelco
Ascentis® Express HILIC, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 15 cm × 2.1 mm
Supelco
Ascentis® Express HILIC, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 10 cm × 3 mm
Supelco
Ascentis® Express HILIC, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 15 cm × 3 mm
Supelco
Ascentis® Express HILIC, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 2 cm × 2.1 mm
Supelco
Ascentis® Express HILIC, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 3 cm × 2.1 mm
Supelco
Ascentis® Express HILIC, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 5 cm × 2.1 mm
Supelco
Ascentis® Express HILIC, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 7.5 cm × 2.1 mm
Supelco
Methanol, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Methanol, Absolute - Acetone free
Sigma-Aldrich
Ammonium formate, reagent grade, 97%
Sigma-Aldrich
Methanol, ACS reagent, ≥99.8%
Sigma-Aldrich
Methanol, ACS reagent, ≥99.8%
Sigma-Aldrich
Methanol, ACS reagent, ≥99.8%
Sigma-Aldrich
Methanol, puriss., meets analytical specification of Ph Eur, ≥99.7% (GC)
Sigma-Aldrich
Methanol, BioReagent, ≥99.93%
Sigma-Aldrich
Heptane, puriss. p.a., reag. Ph. Eur., ≥99% n-heptane basis (GC)
Sigma-Aldrich
Methanol, puriss. p.a., ACS reagent, reag. ISO, reag. Ph. Eur., ≥99.8% (GC)
Sigma-Aldrich
Heptane, ReagentPlus®, 99%
Sigma-Aldrich
Methanol, Laboratory Reagent, ≥99.6%
Prednisolone, British Pharmacopoeia (BP) Assay Standard
Supelco
Ascentis® Express HILIC, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 10 cm × 2.1 mm
Sigma-Aldrich
Heptane, HPLC Plus, for HPLC, GC, and residue analysis, 99%
Sigma-Aldrich
Heptane, suitable for HPLC, ≥99%
Sigma-Aldrich
Methanol, HPLC Plus, ≥99.9%