气相色谱-质谱联用对菠菜中丁烯氟虫腈残留的检测

Study on Determination of Butylene Fipronil Residue in Spinach by Gas Chromatography-Mass Spectrometry

建立了固相萃取(SPE)/气相色谱-质谱(GC-MS)测定菠菜中丁烯氟虫腈残留量的分析方法。利用乙腈提取,提取液依次过无水硫酸钠、氯化钠和PSA固相萃取柱后采用GC-MS进行检测,选择定量离子m/z403,选择定性离子m/z421、55、213、371。6次重复测定峰面积的相对标准偏差小于10%;定量下限为0.05mg/kg,检出限为0.01mg/kg,在0.05～100mg/kg范围内具有良好的线性关系,为丁烯氟虫腈的检测和判断提供了方法。

A method was developed for the determination of butylene fipronil residue in spinach by solid phase extraction （SPE） coupled to gas chromatography- mass spectrometry （GC -MS）. The samples were extracted with acetonitrile and the extract was purified by PSA solid phase extraction col- umn after mixing with Na2 SO4, NaCI in sequence. The detection of butylene fipronil was performed by GC - MS using m/z 421, m/z 55, m/z 213, m/z 371 as qualitative ions and rn/z 403 as quanti- tative ion. A good linearity in the range of 0.05 - 100 mg/kg was obtained for butylene fipronil with the detection limit （S/N = 3 ） of 0. 01 mg/kg and the quantitative limit （S/N = 10） of 0.05 mg/kg. The relative standard deviations（ n = 6） of peak area was lower than 10% . The method was conven- ient, rapid and showed a good reproducibility for detection of butylene fipronil.