Determination of Ethiprole Enantiomers Residue in Rices Using Solid Phase Extraction-Liquid Chromatography Tandem Mass Spectrometry
文献类型: 外文期刊
作者: Zhang Hu 1 ; Qian Ming-Rong 2 ; Wang Xin-Quan 1 ; Liu Fei 3 ; Wang Xiang-Yun 2 ; Xu Hao 2 ; Qi Pei-Pei 2 ; Wang Ming-Hua 1 ;
作者机构: 1.Nanjing Agricultura Univ, Coll Plant Protect, Dept Pesticide Sci, Jiangsu Key Lab Pesticide Sci, Nanjing 210095, Jiangsu, Peoples R China
2.Zhejiang Acad Agr Sci, Inst Qual & Stand Agroprod, Minist Agr, Key Lab Pesticide Residue Detect, Hangzhou 310021, Zhejiang, Peoples R China
3.ThermoFisher Sci Shanghai, Dept Chromatog
关键词: Liquid chromatography tandem mass spectrometry;Ethiprole;Enantiomeric resolution;Rice
期刊名称:CHINESE JOURNAL OF ANALYTICAL CHEMISTRY ( 影响因子:1.134; 五年影响因子:0.909 )
ISSN: 0253-3820
年卷期: 2012 年 40 卷 6 期
页码:
收录情况: SCI
摘要: A simple and sensitive enantioselective method for the determination of ethiprole enantiomers in rice was developed by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Ethiprole was enantioseparated with three cellulose-based chiral stationary phases by HPLC-MS/MS. The effects of the mobile phase and column on the enantiosepartion were studied. The direct resolution of ethiprole enantiomers was performed on a cellulose tris (3, 5-dimethylphenylcarbamate) column (Lux Cellulose-2) using methanol-water (60 : 40, V/V) as mobile phase, and (+)-ethiprole and (-)-ethiprole were eluted and determined by a circular dichroism (CD) detector. The ethiprole residues in rice samples were extracted with acetonitrile and cleaned by NH2 column chromatography.HPLC-MS/MS with electrospray in negative ion scan mode was used to determine ethiprole enantiomers. The fortified recoveries of ethiprole enantiomers in rice matrices including polished rice and brown rice were 87.4%-97.8% at fortification levels ranging from 0.01 to 0.2 mg/kg. Relative standard deviations were 3.1%-9.3%. The limits of quantification for ethiprole enantiomers were both 0.003 mg/kg.
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