固相分散萃取-气相色谱-质谱联用法测定葡萄酒中43种农药残留量

Determination of 43 pesticide residues in grape wine by solid-phase dispersion and gas chromatography-mass spectrometry

中文关键词:  气相色谱-质谱联用法  固相分散萃取  农药  残留检测

英文关键词:gas chromatography-mass spectrometry  solid-phase dispersion  pesticide  residue detection

中文摘要:

      目的 建立固相分散萃取结合气相色谱-质谱联用法(GC/MS)快速测定葡萄酒中敌敌畏、乐果、二嗪磷等葡萄种植过程中常用43种杀虫剂、杀螨剂及杀菌剂残留量。方法 样品用乙腈快速提取、氯化钠和无水硫酸镁盐析后, 经GCB粉、NH2粉和PSA粉组合吸附剂净化, GC/MS外标法定性定量。结果 43种农药在10~500 μg/L范围内线性关系良好, 相关系数R2在0.9851~0.9997范围内, 空白添加浓度在50~200 μg/kg时, 其回收率在67.43%~114.74%之间, 相对标准差(n=6)小于13.6%, 方法的测定下限(LOD)介于1~50 μg/kg之间。 结论 本法简单、准确、快速, 适合于葡萄酒中对43种农药残留量的检测。

英文摘要:

      Objective A rapid analytical method was developed for the determination of 43 pesticide residues in grape wine by solid-phase dispersion with gas chromatography-mass spectrometry (GC/MS). Methods Toally 43 pesticide residues were extracted from the samples with acetonitrile, and then detected by GC/MS with external standard method after being cleaned up with three sorbents (PSA 80.0 mg、GCB 30.0 mg and NH2 30.0 mg). Results Good linearities of 10?500 μg/L were obtained and correlation coefficients were 0.9851?0.9997. The recoveries of all pesticides were in the range from 67.43% to 114.74% at the spiked levels of 50, 100, and 200 μg/kg in grape wine, and the relative standard deviations (RSDs) were not more than 13.6%. The limits of detection (LOD) were 1~50 μg/kg. Conclusion The method could be used for the determination of 43 pesticide residues in grape wine due to its simpleness, accuracy and rapidness.