通过GC和GC-MS方法测定氟吡菌酰胺蔬菜中残留量

Determination of Fluopyram Residues in Vegetables by GC and GC-MS

[目的]建立氟吡菌酰胺在白菜、豇豆和西葫芦3种蔬菜上的气相色谱和气相色谱质谱联用分析方法。[方法]蔬菜样品依次经乙腈提取、N-丙基乙二胺和十八烷基硅烷净化,而后通过气相色谱和气质联用进行定性和定量分析。[结果]氟吡菌酰胺在大白菜、豇豆和西葫芦上的日内和日间试验结果表明:添加质量分数在0.01~1 mg/kg时,氟吡菌酰胺在以上3种蔬菜样品中的平均添加回收率为78.0%~95.2%,相对标准偏差分别为1.3%~7.8%(n=5)和2.2%~6.4%(n=15),最小检出量为0.003 mg/kg,最低检测质量分数为0.01 mg/kg。[结论]该方法简单、快速,准确和精密,能够有效的检测白菜、豇豆和西葫芦上的氟吡菌酰胺的残留量。

[Aims] An accurate method was established to detect the fluopyarm residues in cabbage, cowpea and pumpkin by gas chromatographic with electron capture detector and gas chromatographic-tandem mass chromatographic. [Methods] The samples were extracted with acetonitrile, purified with primary secondary amine （PSA） and octadecylsilane （C18）, and analyzed by gas chromatographic with electron capture detector （GC-μECD） and gas chromatograph- tandem mass spectrometer （GC-MS） via external standard method. [Results] The results showed that when the addition levels were 0.01-1 mg/kg, the average recoveries of fluopyram in cabbage, cowpea and pumpkin were 78.0-95.2%; the relative standard deviations were 1.3-7.8 （n=5） and 2.2-6.4% （n=15）, respectively; the limit of detection （LOD） and the limit of quantification （LOQ） for fluopyram were 0.003 and 0.01 mg/kg, respectively. [Conclusions] The method is simple, rapid and accurate, which can detect the fluopyram residue in cabbage,cowpea and pumpkin.