Determination of residues of kasugamycin and iminoctadine in Orah mandarin using Solid-Phase Extraction/HPLC-MS/MS method
Kasugamycin and iminoctadine tris are commonly used fungicides in Orah production.To set up a method for the simultaneous extraction and determination of kasugamycin and iminoctadine tris residues in Orah fruits using Solid-Phase Extraction(SPE)and High-Performance Liquid Chromatography-Tandem Mass Spectrometry(HPLC-MS/MS),the screening test of extraction agent,the extract purification method,and the liquid chromatography mobile phase system was conducted,and the repeatability and reproducibility of the method were verified.The results showed that the samples were extracted with a 0.2％formic acid aqueous solution,purified with HLB SPE columns,and then interfering substances were removed using strong cation-exchange(SCX)and weak cation-exchange(WCX)SPE columns,respectively.The analysis was performed on a C18-AQ HPLC column in positive electrospray ionization mode with Multiple Reaction Monitoring(MRM).Quantification was conducted using an external standard calibration curve with blank matrix-matched standards,the residues of kasugamycin and iminoctadine can be qualitatively and quantitatively analyzed accurately.There was a good linear relationship between the concentration and peak area of kasugamycin and iminoctadine within the concentration range of 0.005 to 0.500 mg/L,with linear correlation coefficients of 0.9999 and 0.9995,respectively.The method demonstrated high sensitivity,with limits of detection(LOD)of 0.001 mg/kg and limits of quantification(LOQ)of 0.004 mg/kg for both kasugamycin and iminoctadine in Orah.The spiking recoveries ranged from 64.48％to 98.42％for kasugamycin and from 62.38％to 85.86％for iminoctadine.The method showed good repeatability,with relative standard deviations(RSD)of 9.89％and 9.75％for Kasugamycin and Iminoctadine,respectively,across different laboratories.
OrahLiquid Chromatography-Tandem Mass Spectrometrykasugamyciniminoctadine
万方数据
维普
