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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

Sigma-Aldrich
Heptane, SAJ first grade, ≥98.0%
Sigma-Aldrich
Methanol, JIS 300, ≥99.8%, for residue analysis
Sigma-Aldrich
Methanol, SAJ first grade, ≥99.5%
Sigma-Aldrich
Methanol, JIS special grade, ≥99.8%
Sigma-Aldrich
Ammonium formate, SAJ first grade, ≥95.0%
Sigma-Aldrich
Methanol, SAJ special grade
Sigma-Aldrich
Methanol, suitable for HPLC
Supelco
Ibuprofen, Pharmaceutical Secondary Standard; Certified Reference Material
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Prednisolone, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Melting point standard 235-237°C, analytical standard
Sigma-Aldrich
Heptane, JIS special grade, ≥99.0%
Sigma-Aldrich
Methanol, NMR reference standard
Sigma-Aldrich
Methanol, HPLC Plus, ≥99.9%, poly-coated bottles
Supelco
Resorcinol, certified reference material, TraceCERT®, Manufactured by: Sigma-Aldrich Production GmbH, Switzerland
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Benzocaine, Pharmaceutical Secondary Standard; Certified Reference Material
Caffeine for system suitability, European Pharmacopoeia (EP) Reference Standard
Prednisolone for system suitability, European Pharmacopoeia (EP) Reference Standard
Prednisolone, European Pharmacopoeia (EP) Reference Standard
Ibuprofen for peak identification, European Pharmacopoeia (EP) Reference Standard
Supelco
Ascentis® Express HILIC, 5 μm HPLC Column, 5 μm particle size, L × I.D. 10 cm × 4.6 mm
Supelco
Ascentis® Express HILIC, 5 μm HPLC Column, 5 μm particle size, L × I.D. 7.5 cm × 3 mm
Ibuprofen, European Pharmacopoeia (EP) Reference Standard
Supelco
Ascentis® Express HILIC, 5 μm Guard Cartridge, 5 μm particle size, L × I.D. 5 mm × 2.1 mm, pkg of 3 ea
Supelco
Ascentis® Express HILIC, 5 μm Guard Cartridge, 5 μm particle size, L × I.D. 5 mm × 3 mm, pkg of 3 ea
Supelco
Ascentis® Express HILIC, 5 μm HPLC Column, 5 μm particle size, L × I.D. 15 cm × 4.6 mm
Supelco
Ascentis® Express HILIC, 5 μm HPLC Column, 5 μm particle size, L × I.D. 25 cm × 4.6 mm
Supelco
Ascentis® Express HILIC, 5 μm Guard Cartridge, 5 μm particle size, L × I.D. 5 mm × 4.6 mm, pkg of 3 ea
Supelco
Ascentis® Express HILIC, 5 μm HPLC Column, 5 μm particle size, L × I.D. 25 cm × 3 mm
Supelco
Ascentis® Express HILIC, 5 μm HPLC Column, 5 μm particle size, L × I.D. 3 cm × 4.6 mm
Supelco
Ascentis® Express HILIC, 5 μm HPLC Column, 5 μm particle size, L × I.D. 5 cm × 4.6 mm