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Optimization and validation of a fast ultrahigh‐pressure liquid chromatographic method for simultaneous determination of selected sulphonamides in water samples using a fully porous sub‐2 μm column at elevated temperature
Author(s) -
Shaaban Heba,
Górecki Tadeusz
Publication year - 2012
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.201100754
Subject(s) - chromatography , analyte , high performance liquid chromatography , chemistry , detection limit , solid phase extraction , extraction (chemistry) , analytical chemistry (journal) , sample preparation , volumetric flow rate , cartridge , reversed phase chromatography , porosity , phase (matter) , materials science , physics , organic chemistry , quantum mechanics , metallurgy
High temperature in HPLC is considered a valuable tool helping to overcome the increase in the column backpressure when using small packing particles such as sub‐2 μm, as it allows reduction in the mobile‐phase viscosity. In this study, a fast analytical method based on HPLC‐UV was developed using a sub‐2 μm column at elevated temperature for the simultaneous determination of nine sulphonamides. Owing to the lower viscosity of the mobile phase, the separation could be achieved in 3 min at 60°C for all analytes. The effect of temperature, the organic modifier percentage and the flow rate on the retention time was studied. The method developed was used for the determination of selected sulphonamides in surface and wastewater samples. Sample preparation was carried out by solid‐phase extraction on Oasis HLB cartridges. The method developed was validated based on the linearity, precision, accuracy, detection and quantification limits. The recovery ranged from 70.6 to 96 % with standard deviations not higher than 4.7%, except for sulphanilamide. Limits of detection ranged from 1 to 10 μg/L after optimization of all analytical steps. This method has the highest performance in terms of analytical speed compared with other published HPLC‐UV methods for the determination of sulphonamides in water.