气相色谱法检测苹果中氟环唑、咪鲜胺及其代谢物的残留

Determination of epoxiconazole,prochloraz and their metabolites residues in apple by gas chromatography

目的建立气相色谱法检测苹果中咪鲜胺及其代谢物2,4,6-三氯苯酚和氟环唑残留的分析方法。方法匀浆样品加入1%乙酸乙腈振荡,再加入3 g NaCl、2 g无水Na2SO4高速振荡10 min,以5000 r/min离心5 min提取,之后经N-丙基乙二胺(primary secondary amine,PSA)净化,采用气相色谱法进行检测,外标法定量。结果苹果中3种农药在0.01~2.0 mg/L范围内呈良好线性(r2=0.999)。方法定量限为10~20μg/kg。平均回收率为74%~108%,相对标准偏差为2.90%~9.55%。结论该方法准确、快速、可靠,适用于苹果中咪鲜胺及其代谢物2,4,6-三氯苯酚和氟环唑残留量的检测。

Objective To establish a method for the determination of prochloraz and its metabolites 2,4,6-trichlorophenol and epoxiconazole residues in apples by gas chromatography.Methods The homogenate sample was shaken with 1%acetic acid acetonitrile,and then 3g NaCl and 2 g anhydrous Na2 SO4 were added with 10 min shaking at high speed,centrifuged at 5000 r/min for 5 min,then purified with primary secondary amine(PSA),then detected by gas chromatography,and quantified by external standard.Results The linearities of the three pesticides in apple were good in the concentration range from 0.01-2.0 mg/L(r2=0.999),and the limit of quantification was 10-20μg/kg.The average recoveries of three pesticides were in the range of 74%-108%,with relative standard deviations 2.90%-9.55%.Conclusion The method has advantages of accurate,rapid and reliable,which can be used to detect the residue of epoxiconazole,prochloraz and 2,4,6-trichlorophenol in apples.