Determination of Azodicarbonamide in Flour Products by High Performance Liquid Chromatography-Fluorescence Detector Coupled with Precolumn Derivatization

KeyWord:precolumn derivatization  high performance liquid chromatography-fluorescence detector  azodicarbonamide(ADA)  dansyl chloride

Abstract:

      A method was developed for the determination of azodicarbonamide(ADA) in flour products using dansyl chloride(DNS-Cl) precolumn derivatization combined with high performance liquid chromatography-fluorescence detector.ADA in flour products was hydrolyzed by wet heat processing and formed semicarbazide(SEM) finally.SEM was derivatized with DNS-Cl.The derivatization product was separated on an Aglient TC C18 column(250 mm¡Á¡¡4.6 mm,5 ¦Ìm) using acetonitrile-water(65¡Ã35) as mobile phase at a flow rate of 1.0 mL/min.The oven temperature was set at 30 ¡æ£¬the excitation wavelength was 330 nm and the detection wavelength was 530 nm.Under the optimal conditions,the linear range for ADA was in the range of 0.1-50 mg/L with correlation coefficient(r) higher than 0.998.The limits of detection(LOD)and limits of quantitation(LOQ) for the method were 0.03 mg/L and 0.10 mg/L,respectively.The spiked recoveries of ADA at three levels of 0.1,0.3,1.0 mg/kg ranged from 78.4%to 96.6%with RSDs of 7.1%-9.4%.With advantages of simplicity,rapidness and sensitivivity,the method was successfully applied in the analysis of ADA in flour products.