Determination of sulfonamides in swine muscle after salting-out assisted liquid extraction with acetonitrile coupled with back-extraction by a water/acetonitrile/dichloromethane ternary component system prior to high-performance liquid chromatography

A salting-out assisted liquid extraction coupled with back-extraction by a water/acetonitrile/dichloromethane ternary component system combined with high-performance liquid chromatography with diode-array detection (HPLC–DAD) was developed for the extraction and determination of sulfonamides in solid tissue samples. After the homogenization of the swine muscle with acetonitrile and salt-promoted partitioning, an aliquot of 1 mL of the acetonitrile extract containing a small amount of dichloromethane (250–400 μL) was alkalinized with diethylamine. The clear organic extract obtained by centrifugation was used as a donor phase and then a small amount of water (40–55 μL) could be used as an acceptor phase to back-extract the analytes in the water/acetonitrile/dichloromethane ternary component system. In the back-extraction procedure, after mixing and centrifuging, the sedimented phase would be water and could be withdrawn easily into a microsyringe and directly injected into the HPLC system. Under the optimal conditions, recoveries were determined for swine muscle fortified at 10 ng/g and quantification was achieved by matrix-matched calibration. The calibration curves of five sulfonamides showed linearity with the coefficient of estimation above 0.998. Relative recoveries for the analytes were all from 96.5 to 109.2% with relative standard deviation of 2.7–4.0%. Preconcentration factors ranged from 16.8 to 30.6 for 1 mL of the acetonitrile extract. Limits of detection ranged from 0.2 to 1.0 ng/g.