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  • On-line hyphenation of solid-phase extraction to chromatographic separation of sulfonamides with fused-core columns in sequential injection chromatography.

On-line hyphenation of solid-phase extraction to chromatographic separation of sulfonamides with fused-core columns in sequential injection chromatography.

Talanta (2014-12-02)
Alex D Batista, Petr Chocholouš, Dalibor Satínský, Petr Solich, Fábio R P Rocha
ABSTRACT

On-line sample pretreatment (clean-up and analyte preconcentration) is for the first time coupled to sequential injection chromatography. The approach combines anion-exchange solid-phase extraction and the highly effective pentafluorophenylpropyl (F5) fused-core particle column for separation of eight sulfonamide antibiotics with similar structures (sulfathiazole, sulfanilamide, sulfacetamide, sulfadiazine, sulfamerazine, sulfadimidine, sulfamethoxazole and sulfadimethoxine). The stationary phase was selected after a critical comparison of the performance achieved by three fused-core reversed phase columns (Ascentis(®) Express RP-Amide, Phenyl-Hexyl, and F5) and two monolithic columns (Chromolith(®) High Resolution RP-18 and CN). Acetonitrile and acetate buffer pH 5.0 at 0.60 mL min(-1) were used as mobile phase to perform the separations before spectrophotometric detection. The first mobile phase was successfully used as eluent from SPE column ensuring transfer of a narrow zone to the chromatographic column. Enrichment factors up to 39.2 were achieved with a 500 µL sample volume. The developed procedure showed analysis time <10.5 min, resolutions >1.83 with peak symmetry ≤1.52, LODs between 4.9 and 27 µg L(-1), linear response ranges from 30.0 to 1000.0 µg L(-1) (r(2)>0.996) and RSDs of peak heights <2.9% (n=6) at a 100 µg L(-1) level and enabled the screening control of freshwater samples contaminated at the 100 µg L(-1) level. The proposed approach expanded the analytical potentiality of SIC and avoided the time-consuming batch sample pretreatment step, thus minimizing risks of sample contamination and analyte losses.

MATERIALS
Product Number
Brand
Product Description

Supelco
Ascentis® Express F5, 5 μm Guard Cartridge, 5 μm particle size, L × I.D. 5 mm × 4.6 mm, pkg of 3 ea
Supelco
Ascentis® Express F5, 5 μm HPLC Column, 5 μm particle size, L × I.D. 25 cm × 2.1 mm
Supelco
Ascentis® Express F5, 5 μm HPLC Column, 5 μm particle size, L × I.D. 3 cm × 3 mm
Supelco
Ascentis® Express F5, 5 μm HPLC Column, 5 μm particle size, L × I.D. 25 cm × 4.6 mm
Supelco
Ascentis® Express F5, 5 μm HPLC Column, 5 μm particle size, L × I.D. 7.5 cm × 3 mm
Supelco
Ascentis® Express F5, 5 μm Guard Cartridge, 5 μm particle size, L × I.D. 5 mm × 2.1 mm, pkg of 3 ea
Supelco
Ascentis® Express F5, 5 μm HPLC Column, 5 μm particle size, L × I.D. 2 cm × 2.1 mm
Supelco
Ascentis® Express F5, 5 μm HPLC Column, 5 μm particle size, L × I.D. 10 cm × 3 mm
Supelco
Ascentis® Express F5, 5 μm HPLC Column, 5 μm particle size, L × I.D. 15 cm × 3 mm
Supelco
Ascentis® Express F5, 5 μm HPLC Column, 5 μm particle size, L × I.D. 25 cm × 3 mm
Supelco
Ascentis® Express F5, 5 μm HPLC Column, 5 μm particle size, L × I.D. 5 cm × 3 mm
Supelco
Ascentis® Express F5, 5 μm HPLC Column, 5 μm particle size, L × I.D. 10 cm × 2.1 mm
Supelco
Ascentis® Express F5, 5 μm HPLC Column, 5 μm particle size, L × I.D. 5 cm × 4.6 mm
Supelco
Ascentis® Express F5, 5 μm Guard Cartridge, 5 μm particle size, L × I.D. 5 mm × 3 mm, pkg of 3 ea
Supelco
Ascentis® Express Phenyl-Hexyl, 2.7 μm HPLC Column, 2.7 μm particle size, L × I.D. 7.5 cm × 2.1 mm
Supelco
Ascentis® Express Phenyl-Hexyl, 2.7 μm HPLC Column, 2.7 μm particle size, L × I.D. 7.5 cm × 4.6 mm
Supelco
Ascentis® Express Phenyl-Hexyl, 2.7 μm HPLC Column, 2.7 μm particle size, L × I.D. 10 cm × 4.6 mm
Supelco
Ascentis® Express Phenyl-Hexyl, 2.7 μm HPLC Column, 2.7 μm particle size, L × I.D. 7.5 cm × 3 mm
Supelco
Ascentis® Express Phenyl-Hexyl, 2.7 μm HPLC Column, 2.7 μm particle size, L × I.D. 15 cm × 3 mm
Supelco
Ascentis® Express Phenyl-Hexyl, 2.7 μm HPLC Column, 2.7 μm particle size, L × I.D. 2 cm × 2.1 mm
Supelco
Ascentis® Express Phenyl-Hexyl, 2.7 μm Guard Cartridge, 2.7 μm particle size, L × I.D. 5 mm × 2.1 mm, pkg of 3 ea
Supelco
Ascentis® Express Phenyl-Hexyl, 2.7 μm Guard Cartridge, 2.7 μm particle size, L × I.D. 5 mm × 4.6 mm, pkg of 3 ea
Supelco
Ascentis® Express Phenyl-Hexyl, 2.7 μm Guard Cartridge, 2.7 μm particle size, L × I.D. 5 mm × 3 mm, pkg of 3 ea
Supelco
Ascentis® ES-Cyano HPLC Column, 5 μm particle size, L × I.D. 15 cm × 4.6 mm
Supelco
Ascentis® ES-Cyano HPLC Column, 5 μm particle size, L × I.D. 10 cm × 2.1 mm
Supelco
Ascentis® Express Phenyl-Hexyl, 2.7 μm HPLC Column, 2.7 μm particle size, L × I.D. 5 cm × 2.1 mm
Supelco
Ascentis® Express Phenyl-Hexyl, 2.7 μm HPLC Column, 2.7 μm particle size, L × I.D. 3 cm × 2.1 mm
Supelco
Ascentis® Express Phenyl-Hexyl, 2.7 μm HPLC Column, 2.7 μm particle size, L × I.D. 3 cm × 3 mm
Supelco
Ascentis® Express Phenyl-Hexyl, 2.7 μm HPLC Column, 2.7 μm particle size, L × I.D. 3 cm × 4.6 mm
Supelco
Ascentis® Phenyl HPLC Column, 5 μm particle size, L × I.D. 25 cm × 4.6 mm