固相萃取-气相色谱法测定果汁中多种农药残留

Determination of pesticides multi-residues in juice by solid phase extraction-gas chromatography

中文关键词:  果汁  固相萃取  气相色谱法  火焰光度检测器  电子捕获检测器  农药残留

英文关键词:juice  solid phase extraction  gas chromatography  flame photometric detector  electron capture detector  pesticides residues

中文摘要:

      目的 建立QuEChERS提取盐包及固相萃取净化技术结合气相色谱法测定果汁中17种农药(敌敌畏、甲胺磷、乙酰甲胺磷、甲拌磷、氧乐果、乐果、毒死蜱、杀螟硫磷、水胺硫磷、三唑磷、联苯菊酯、甲氰菊酯、氯氟氰菊酯、氯氰菊酯、氟氰戊菊酯、氰戊菊酯、溴氰菊酯)残留的分析方法。方法 果汁样品经乙酸乙酯及QuEChERS提取包提取, 提取液通过石墨化碳黑净化, 以气相色谱火焰光度检测器(flame photometric detector, FPD)、电子捕获检测器(electron capture detector, ECD)检测, 外标法定量。结果 10种有机磷农药在0.020~0.15 mg/L及7种拟除虫菊酯类农药在0.01~0.1 mg/L浓度范围内线性关系良好(r2≥0.9991), 方法的检出限(limits of detection, LOD)均在0.023 mg/kg以下, 平均加标回收率为72.7%~115.0%之间, 相对标准偏差(relative standard deviation, RSD)均小于5.84%。结论 本方法具有灵敏、简便、稳定, 可以满足果汁样品中多种农药残留的检测要求。

英文摘要:

      Objective To establish an analysis method for determination of 17 kinds of pesticides (dichlorvos, methamidophos, acephate, phorate, omethoate, dimethoate, chlorpyrifos, fenitrothion, isocarbophos, triazophos, bifenthrin, fenpropathrin, cyhalothrin, cypermethrin, flucythrinate, fenvalerate, deltamethrin, etc) residues in juice by the QuEChERs extraction salt package and solid phase extraction-gas chromatography (GC). Methods Juice samples were extracted with ethyl acetate and QuEChERs extraction salt package, and the extract was purified by graphitized carbon black. Analytes were detected with gas chromatography (GC)–flame photometric detector (FPD) and gas chromatography (GC)–electron capture detector (ECD), external standard method for quantitative. Results Ten kinds of organophosphorus pesticides and 7 kinds of pyrethroid pesticides had good linear relationships in the range of 0.020-0.15 mg/L and 0.01-0.1 mg/L, respectively (r2≥0.9991). The limits of detection (LODs) for the 17 kinds of pesticides were below 0.023 mg/kg; The recoveries were ranged from 72.7% to 115.0%, with the relative standard deviations (RSDs) were less than 5.84% (n=6). Conclusion This method is sensitive, simple and reliable, which is suitable for detecting multiple pesticides residues in juice samples.