QuEChERS-气相色谱法测定甜豆中3种农药残留

作者:刘金;姬春红;曾东强;刘晓亮; 刊名:农药 上传者:邓克平

【摘要】[目的]建立QuEChERS-气相色谱法(GC)快速准确测定甜豆全果和豆荚中毒死蜱、联苯菊酯和高效氯氟氰菊酯3种农药残留的方法。[方法]采用QuEChERS前处理的方法对样品进行净化处理,即甜豆全果和荚中毒死蜱、联苯菊酯、高效氯氟氰菊酯经乙腈高速涡旋提取,上清液经无水硫酸镁和N-丙基乙二胺(PSA)、石墨化炭黑(GCB)净化后过有机膜进行气相色谱电子捕获检测器(ECD)检测,以基质匹配标准溶液外标法定量。[结果] 3种农药的线性相关系数均不低于0.997,在0.01、0.1、1 mg/L的添加水平下,3种农药在甜豆全果基质、豆荚中方法回收率在75%~102%范围内,相对标准偏差(RSD)在1%~11%范围内,方法定量限(LOQ)为0.01 mg/L。[结论]该方法前处理简单快速、灵敏度高,适用于甜豆中毒死蜱、联苯菊酯、高效氯氟氰菊酯的检测。

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QuEChERS-气相色谱法测定甜豆中3种农药残留 刘 金,姬春红,曾东强,刘晓亮 (广西大学 农药与环境毒理研究所,南宁 530005) 摘要: [目的]建立QuEChERS-气相色谱法(GC)快速准确测定甜豆全果和豆荚中毒死蜱、联苯菊酯和高效氯氟氰菊酯3种农药残留的方法。[方法]采用QuEChERS前处理的方法对样品进行净化处理,即甜豆全果和荚中毒死蜱、联苯菊酯、高效氯氟氰菊酯经乙腈高速涡旋提取,上清液经无水硫酸镁和N- 丙基乙二胺(PSA)、石墨化炭黑(GCB)净化后过有机膜进行气相色谱电子捕获检测器(ECD)检测,以基质匹配标准溶液外标法定量。[结果] 3种农药的线性相关系数均不低于0.997,在0.01、0.1、1 mg/L的添加水平下,3种农药在甜豆全果基质、豆荚中方法回收率在75%~102%范围内,相对标准偏差(RSD)在1%~11%范围内,方法定量限(LOQ)为0.01 mg/L。[结论]该方法前处理简单快速、灵敏度高,适用于甜豆中毒死蜱、联苯菊酯、高效氯氟氰菊酯的检测。关键词:甜豆;气相色谱;农药残留;QuEChERS 中图分类号:TQ450.2 文献标志码:A 文章编号:1006-0413(2019)02-0118-03 Determination of Three Pesticide Residues in Baked Bean by QuEChERS- Gas Chromatography LIU Jin, JI Chun- hong, ZENG Dong- qiang, LIU Xiao- liang (Institute of Pesticide and Environmental Toxicology, Guangxi University, Nanning 530005, China) Abstract:[Aims] A rapid and accurate method was developed for the analysis of three pesticide residues in baked bean based on gas chromatography(GC). [Methods] By modified QuEChERS method, chlorpyrifos, bifenthrin and lambda-cyhalothrin residues in baked bean samples were extracted with acetonitrile, cleaned up with MgSO4 and primary secondary amine (PSA) and graphitized carbon black (GCB), then detected by GC-ECD.The quantatative method was established using the matrix-matched calibration standards as the external standard. [Results] The results indicated that the linear correlation coefficients (R2) were no less than 0.997 with relative standard deviations (RSD) of 1-11%, the limits of quantitation was 0.01 mg/kg.The

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