QuEChERS-气相色谱法测定甜豆中3种农药残留
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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。
[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 Mg SO4 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) of1-11%, the limits of quantitation was 0.01 mg/kg.The recoveries of 3 pesticides at three spiked concentration levels ranged from 75 to 102%. [Conclusions] The method is simple, rapid, accurate and sensitive, and is appropriate for the determination of 3 pesticide residues in baked bean.
[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 Mg SO4 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) of1-11%, the limits of quantitation was 0.01 mg/kg.The recoveries of 3 pesticides at three spiked concentration levels ranged from 75 to 102%. [Conclusions] The method is simple, rapid, accurate and sensitive, and is appropriate for the determination of 3 pesticide residues in baked bean.
引文
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[10]曹小丽,刘素华,刘仲,等.气相色谱-串联质谱结合QuEChERS方法检测蔬菜、水果中62种农药残留[J].中国卫生检验杂志,2015,25(8):1119-1124.
[11]叶倩,邓义才,路大海,等.气相色谱法测定蔬菜水果中氟虫腈等6种农药残留[J].农药,2016,55(1):51-54.
[2]马云昆.安宁市小荷兰豆与甜豆无公害栽培技术[J].现代农业科技,2018(10):64-66.
[3]杨文迪.改进QuEChERS技术结合LC-MS/MS测定果蔬中农药多残留(硕士论文)[D].泰安:山东农业大学,2017.
[4]武晓丽.几种纳米材料在农药残留和有机污染物分析方面的应用(博士论文)[D].北京:中国农业大学,2017.
[5]杨珂.苦瓜和黄瓜中农药多残留检测方法及几种杀菌剂残留消解动态研究(硕士论文)[D].南宁:广西大学,2017.
[6]吴丹亚,陈芹,潘洁.宁波市常见根茎类蔬菜农药残留分析[J].浙江农业科学,2017,58(5):850-852.
[7]姚勇,刘全科.2015年湖北省蔬菜有机磷农药残留分析[J].湖北农业科学,2016,55(20):5352-5354.
[8]张婷,李满秀,贾海清,等.LC-MS/MS法测定大棚蔬菜氨基甲酸酯类农药残留分析研究[J].海南师范大学学报(自然科学版),2016,29(4):414-417.
[9]王世英.鱼藤酮和呋虫胺在多种蔬菜中的消解规律及影响因素研究(硕士论文)[D].广州:华南农业大学,2016.
[10]曹小丽,刘素华,刘仲,等.气相色谱-串联质谱结合QuEChERS方法检测蔬菜、水果中62种农药残留[J].中国卫生检验杂志,2015,25(8):1119-1124.
[11]叶倩,邓义才,路大海,等.气相色谱法测定蔬菜水果中氟虫腈等6种农药残留[J].农药,2016,55(1):51-54.