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

作　　者：李敏青 庄嘉 徐娟[1,2] 王岚 安文佳[1,2] 孙灵慧 LI Min-Qing;ZHUANG Jia;XU Juan;WANG Lan;AN Wen-Jia;SUN Ling-Hui(Inspection &Quarantine Technology Center of Guangdong Entry-Exit Inspection and Quarantine Bureau,Guangzhou 510623,China;Guangdong Key Laboratory of Import and Export Technical Measures of Animal,Plant and Food,Guangzhou 510623,China)

机构地区：[1]广东出入境检验检疫局检验检疫技术中心,广州510623 [2]广东省动植物与食品进出口技术措施研究重点实验室,广州510623

出　　处：《食品安全质量检测学报》2018年第24期6508-6514,共7页Journal of Food Safety and Quality

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)、甴子捕获检测器(electron capture detector, ECD)检测,外标法定量。结果 10种有机磷农药在0.020～0.15mg/L及7种拟除虫菊酯类农药在0.01～0.1mg/L浓度范围内线性关系良好(r^2≥0.9991),方法的检出限(limits of detection,LOD)均在0.023mg/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。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 7kinds 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 (r^2≥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.

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 

分 类 号：TS255.44[轻工技术与工程—农产品加工及贮藏工程] O657.71[轻工技术与工程—食品科学与工程]