Tolerance intervals modeling for design space of a salt assisted liquid-liquid microextraction of trimethoprim and six common sulfonamide antibiotics in environmental water samples
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Abstract
Sulfonamides and trimethoprim combinations have been used extensively as antimicrobial
agents for prevention and treatment of human and animal infections. Although many
microextraction methods were developed for monitoring their residues in environmental
water, none of these methods applied liquid-liquid microextraction for this purpose.
This work presents for the first time a simultaneous Salt Assisted Liquid-Liquid Microextraction
SALLME coupled with HPLC-UV for determination of trimethoprim and six common sulfonamide
residues (sulfathiazole, sulfadiazine, sulfadmidine, sulfamethoxazole sulfadoxine
and sulfaquinoxaline) in water samples. Co-extraction of trimethoprim with sulfonamides
was achieved by the addition of perchloric acid as a chaotropic agent to the extraction
medium. Quality by Design framework was applied to develop and optimize both of SALLME
and HPLC steps to ensure procedure robustness and sensitivity. Tolerance interval
modeling of SALLME responses was applied to construct the design space of SALLME procedure.
The optimized HPLC system enabled fast, sensitive and robust separation the extracted
compounds within four minutes. The method detection limits of the method were in the
range of 2.15-7.64 ng.mL-1. These values were far below the guidelines recommended
limits (35 and 70 ng.mL-1 for each individual sulfonamide and trimethoprim respectively).