衍生化-气相色谱法测定谷物籽粒中三氯吡氧乙酸残留量  

Determination of triclopyr residue in cereal seeds by gas chromatography with derivatization

作　　者：杨亚琴[1] 李圆圆[1] 曹秀[1] 刘燕 冯慧慧 余明霞 卫艳利 李淑芳[1] 冯书惠[1] 郝学飞[1] YANG Yaqin;LI Yuanyuan;CAO Xiu;LIU Yan;FENG Huihui;YU Mingxia;WEI Yanli;LI Shufang;FENG Shuhui;HAO Xuefei(Institute of Agro-product Quality and Safety,Henan Academy of Agricultural Sciences,Zhengzhou 450002,China;Henan Institute of Product Quality Supervision and Inspection,Zhengzhou 450007,China;Seed Industry Development Center of Mengjin District,Luoyang 471100,Henan,China)

机构地区：[1]河南省农业科学院农产品质量安全研究所,郑州450002 [2]河南省产品质量监督检验院,郑州450007 [3]洛阳市孟津区种业发展中心,河南洛阳471100

出　　处：《农药》2024年第3期191-195,227,共6页Agrochemicals

基　　金：河南省农业科学院自主创新专项基金项目(2021ZC63);河南省农业科学院优秀青年科技基金计划项目(2022YQ29);河南省市场监督管理局科技攻关计划项目(2021sj25)。

摘　　要：[目的]建立一种衍生化-气相色谱法测定谷物籽粒中三氯吡氧乙酸的分析方法。[方法]样品采用1%乙酸乙腈提取,于水浴中减压蒸发及常温下氮气吹干后,用丙酮复溶。复溶液经14%三氟化硼甲醇溶液于60℃衍生化反应60 min后,正己烷萃取衍生物,电子捕获检测器-气相色谱仪检测,外标法定量。[结果]在0.01~2.0 mg/L范围内,三氯吡氧乙酸衍生化产物的峰面积与质量浓度呈现良好的线性关系,相关系数r为0.9997。在添加质量分数为0.01~1.0 mg/kg时,小麦、大米、小米、玉米不同谷物籽粒基质中三氯吡氧乙酸的平均回收率在80.7%~101%,相对标准偏差RSD为1.42%~9.05%(n=5),方法的定量限均为0.01 mg/kg。[结论]该分析方法将三氯吡氧乙酸经酸性乙腈提取、甲酯化衍生后气相色谱测定,灵敏度高、准确度好,符合农药残留检测分析要求,可应用于谷物籽粒中三氯吡氧乙酸的残留监测。[Aims] This study aims to establish a method of gas chromatography with derivatization for the quantitative determination of triclopyr residue in cereal seeds. [Methods] Triclopyr was extracted by acetonitrile with1% acetic acid. The extracted solution was evaporated under reduced pressure in water bath and dried with nitrogen at room temperature. The extract was dissolved in acetone, and then reacted with 14% boron trifluoride in methanol at60 ℃ for 60 min. The derivative was extracted with n-hexane, detected by the gas chromatography coupled with electron capture detector(GC-ECD) and quantified by an external standard method. [Results] In the concentration range from 0.01 to 2.0 mg/L, the peak area values of triclopyr derivative showed good linearity with coefficient(r) of0.9997. At the spiked levels from 0.01 to 1.0 mg/kg, the average recoveries of triclopyr in wheat, rice, millet and maize were in the range of 80.7%-101%, with the relative standard deviations(RSDs) of 1.42%-9.05%(n=5). The limit of quantification(LOQ) for triclopyr was 0.01 mg/kg in cereal seeds. [Conclusions] Triclopyr can be extracted by acetonitrile with acetic acid, derived to methyl ester and detected by GC-ECD. The proper analytical method has well separation, high sensitivity and good accuracy. It meets the requirements of pesticide residue analysis for monitoring the residue of triclopyr in cereal seeds.

关 键 词：衍生化 气相色谱 三氯吡氧乙酸 谷物籽粒 

分 类 号：TQ450.2[化学工程—农药化工]