SPE-GC-MS/MS法检测铁皮石斛中5种三唑类农药的残留量

SPE-GC/MS/MS method for determination 5 triazole pesticide residues in dendrobium officinale

目的建立固相萃取样品,采用气相色谱-串联质谱(GC-MS/MS)联用技术检测铁皮石斛中5种三唑类(三唑酮、三唑醇、烯唑醇、戊唑醇和腈苯唑)农药残留量的分析方法。方法铁皮石斛样品粉碎后,用乙腈萃取,HLB固相萃取柱净化,1 mL丙酮溶解残渣并经0.45μm滤膜过滤后,GC-MS/MS法进样分析。结果5种三唑类农药残留在0.05~5.0μg/mL质量浓度范围内线性良好,线性相关系数均大于0.995,检出限均在0.012~0.020 mg/kg之间,3个不同浓度点的加样回收率均在82.6%~99.8%之间,重复性与精密度试验RSD值(n=6)均小于5.0%,溶液24 h内稳定。结论该方法前处理简单,灵敏度与准确度较高,适用于铁皮石斛中三唑类农药残留的监测。

Objective To establish a SPE-GC/MS/MS method for determination five triazole pesticide(triazolone,triadimenol,diniconazole,tebuconazole and fenethanil)residues in dendrobium officinale.Methods Samples were crushed and extracted with acetonitrile,and then purified by HLB solid phase extraction column.1 mL acetone was used to dissolve residue and filtered by 0.45μm filter membrane.Samples were analyzed by GC-MS/MS.Results Five triazole pesticides showed good linear relationship in the range 0.05-5.0μg/mL,and the correlation coefficients(r)were all above 0.995.Detection limits were in the range 0.012-0.020 mg/kg.Recoveries in three different concentrations were in the range 82.6%-99.8%.RSD of repeatability and precision were all less than 5.0%,and the solution was stable within 24 hours.Conclusion This method has the advantages of simple pretreatment,high sensitivity and accuracy,which is suitable for the detection of triazole pesticide residues in dendrobium officinalis.