分析化学2011，Vol.39Issue(1)：72-76,5.
固相萃取-全二维气相色谱/飞行时间质谱同步快速检测蔬菜中64种农药残留
Rapid Screening and Simultaneous Confirmation of 64 Pesticide Residues in Vegetable Using Solid Phase Extraction-comprehensive Two-dimensional Gas Chromatography Coupled with Time-of-Flight Mass Spectrometer
摘要
Abstract
A solid phase extraction-comprehensive two-dimensional gas chromatography coupled with time-of-flight mass Spectrometric (GC× GC-TOF-MS) method for analysis of 64 pesticides in vegetables was developed and validated. After extracting with acetonitrile, cleaning-up with NH2-SPE cartridge and concentrating with nitrogen, the pesticide residues were redissolved in the acetone and analyzed by GC × GC-TOF-MS coupled with HP-5MS and column DB-17 column. Sample matrixmatched calibration was used to determine the residue contents by external standard. The method was validated by the real samples, such as Brassica campestris, cucumber, eggplant, kidney bean and capsicum. The limits of detection (S/N=3) and the limits of quantification (S/N= 10) were from 0.010 to 6. 032 μg/kg and from 0. 035 to 20. 107 tg/kg, respectively. The overall recoveries ranged from 68.3％ to 117.8％ with the relative standard deviations (RSD) of 0. 6％-9.1％. Two positive samples, polluted by acephate and cypermethrin with a residual concentration of 0. 036 and 0. 107 mg/kg, were screened by the developed method as detecting markets samples.关键词
全二维气相色谱-飞行时间质谱/农药残留/蔬菜Key words
Comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry/Multiple pesticide residues/ Vegetable引用本文复制引用
姜俊,李培武,谢立华,丁小霞,李英,王秀嫔,汪雪芳,张奇,管笛..固相萃取-全二维气相色谱/飞行时间质谱同步快速检测蔬菜中64种农药残留[J].分析化学,2011,39(1):72-76,5.基金项目
本文系国家科技支撑计划(No.2009BADB9B03-Z09)和武汉市青年科技晨光计划(No.200950431224)资助 （No.2009BADB9B03-Z09）
