基质固相分散-气相色谱检测菊花中有机磷农药残留

Determination of Organophosphorus Pesticide Residues in Flos Chrysanthemi by Matrix Solid Phase Dispersion-Gas Chromatography

建立菊花中14种有机磷农药残留量的气相色谱分析方法。样品用乙腈-丙酮(4:1,V/V)提取,经基质固相分散技术净化,以乙腈-甲苯(3:1,V/V)洗脱,气相色谱-火焰光度检测,外标法定量。在0.05～1.0mg/kg的添加水平,14种有机磷的平均回收率在84.54%～108.54%之间,相对标准偏差在0.66%～6.31%,该方法的检出限为0.01～0.04mg/kg。该方法的灵敏度、准确度和精密度均符合农药残留测定的技术要求。采用所建立方法测定了黄山贡菊、杭白菊和胎菊3种代表性菊花中14种有机磷农药残留量,结果表明,黄山贡菊检出乐果1.68mg/kg、毒死蜱0.17mg/kg、硫环磷0.28mg/kg,杭白菊检出毒死蜱0.09mg/kg,胎菊检出乐果0.25mg/kg、毒死蜱0.14mg/kg、伏杀磷0.08mg/kg。

An analytical method was developed for the simultaneous determination of 14 organophosphorus pesticides in Flos Chrysanthemi by using matrix solid phase dispersion （MSPD） and gas chromatography （GC）. Flos Chrysanthemi samples were extracted with acetonitrile-acetone （4：1, V/V） and cleaned up by mallix solid phase dispersion （MSPD）, eluted with acetonitrUe toluene （3：1, V/V） and determined by GC with a flame photometric detector. The recovery rates of 14 organophosphorus pesticides were 84.54%～ 108.54% with relative standard deviation of 0.66% - 6.31% at spiked levels of 0.05 - 1.0 mg/kg. The limit of detection was 0.01 -- 0.04 mg/kg. The proposed method was characterized by simplicity, higher sensitivity and accuracy. The contents of dimethoate, chlorpyrifos and phosfolan in Huangshan Gongju chrysanthemum were 1.68, 0.17 mg/kg and 0.28 mg/kg, respectively, the content of chlorpyrifos in Hangbaiju chrysanthemum was 0.09 mg/kg, and the contents of dimethoate, chlorpyrifos and phosalone in Hangbalju chrysanthemum bud were 0.25, 0.14 mg/kg and 0.08 mg/kg, respectively as determined by this method.