Determination of 18 Sulfonamide Residues in Pork by Modified QuEChERS/HPLC with Online Photochemical Derivatization and Fluorescence Detection
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Determination of 18 Sulfonamide Residues in Pork by Modified QuEChERS/HPLC with Online Photochemical Derivatization and Fluorescence Detection
Vol. 34, Issue 7, Pages: 807-812(2015)
作者机构:
1. 中国科学院西北高原生物研究所
2. 中国科学院大学
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Determination of 18 Sulfonamide Residues in Pork by Modified QuEChERS/HPLC with Online Photochemical Derivatization and Fluorescence Detection. [J]. 34(7):807-812(2015)
DOI:
Determination of 18 Sulfonamide Residues in Pork by Modified QuEChERS/HPLC with Online Photochemical Derivatization and Fluorescence Detection. [J]. 34(7):807-812(2015)DOI:
Determination of 18 Sulfonamide Residues in Pork by Modified QuEChERS/HPLC with Online Photochemical Derivatization and Fluorescence Detection
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×250 mm,5 μm),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 ℃,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 μg?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 μg/kg to 18 μg/kg,the limits of quantitation(S/N=10) were in the range of 3-60 μg?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.
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Simultaneous Determination of Xylazine and Its Metabolite 2,6-Dimethylaniline in Pork by QuEChERS/Liquid Chromatography-Tandem Mass Spectrometry
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