Determination of 18 Sulfonamide Residues in Pork by Modified QuEChERS/HPLC with Online Photochemical Derivatization and Fluorescence Detection

KeyWord:pork  sulfonamides  QuEChERS  online photochemical derivatization  HPLC/FLD

Abstract:

      A method was developed for the determination of 18 sulfonamide residues in pork by using modified QuEChERS/high performance liquid chromatography with online post column photochemical derivatization and fluorescence detector.The residues in the samples were extracted with 1% acetic acid acetonitrile solution,cleaned by QuEChERS£¨Quick,Easy,Cheap,Effective,Rugged and Safe) method using a mixture of PSA£¬C18 and GCB as sorbent.The target compounds were separated by HPLC on a Platisil ODS column£¨4.6 mm¡Á250 mm,5 ¦Ìm),and then treated by on-line photochemical derivatization and detected with a fluorescence detector.The optimal conditions were as follows:excitation wavelength:320 nm,emission wavelength:450 nm, column temperature: 36 ¡æ,mobile phase:0.3% acetic acid-methanol by gradient elution.Under the optimized conditions,a good baseline separation of 18 analytes was obtained.The calibration curves were linear in the range of 0.05-110.28 ¦Ìg?mL-1 for 18 sulfonamides,with correlation coefficients£¨r) larger than 0.992 0 .The method detection limits(S/N=3) for target compounds ranged from 1 ¦Ìg/kg to 18 ¦Ìg/kg,the limits of quantitation£¨S/N=10) were in the range of 3-60 ¦Ìg?kg-1.The spiked recoveries of 18 sulfonamide residues varied from 71.2% to 113.4%,in which the majority recoveries were in the range of 80%-100%.The relative standard deviations(RSDs) were 0.8%-8.7%.The method showed advantages of rapidness,simplicity, less organic solvents,reliability,good accuracy and precision,and could meet the requirements for qualification and quantification analysis of 18 sulfonamide residues in pork.