摘要
建立干木耳中有机氯及拟除虫菊酯类农药残留气相色谱测定方法,为广大质检机构开展干木耳中农药残留检测提供参考。样品中有机氯及拟除虫菊酯类农药经乙腈提取,提取液经水浴蒸发浓缩,正己烷定容,气相色谱-电子捕获法测定,并通过验证试验对方法的可行性、科学性及准确性等进行评价。结果表明:该方法条件下,各农药线性关系良好,相关系数均大于0.99;方法定量限为0.002~0.02 mg·kg^(-1);测定结果的RSD值(n=6)为1.77%~11.17%;0.02 mg·kg^(-1)和0.05 mg·kg^(-1)添加水平的回收率为74.0%~110.5%,0.25 mg·kg^(-1)添加水平的回收率为79.0%~102.3%;17种农药中,有14种农药的ME值小于0.85,存在基质负效应,需要考虑基质效应的影响。综上,该分析测试方法灵敏度高、精密度和准确性好,且成本低廉、操作简单、适用范围广,便于广大质检机构参考应用。
To establish a gas chromatography method for the determination of organochlorine and pyrethroid pesticide residues in dried Auricularia,providing reference for quality inspection institutions to carry out pesticide residue detection in dried Auricularia.The organic chlorine and pyrethroid pesticides in the sample were extracted with acetonitrile.The extract was evaporated and concentrated in a water bath,and the volume of n-hexane was determined by gas chromatography-electron capture method.The feasibility,scientificity,and accuracy of the method were evaluated through validation experiments.The results indicate that under the conditions of this method,the linear relationship of each pesticide was good,and the correlation coefficients were all greater than 0.99.The quantitative limit of the method was between 0.002 mg·kg^(-1)and 0.02 mg·kg^(-1).The RSD value of the measurement result(n=6)was between 1.77%and 11.17%.The recovery rates of 0.02 mg·kg^(-1)and 0.05 mg·kg^(-1)addition levels ranged from 74.0%to 110.5%,while the recovery rates of 0.25 mg·kg^(-1)addition levels ranged from 79.0%to 102.3%.Among the 17 pesticides,14 had a ME value less than 0.85,indicating a negative matrix effect,which needed to be considered.In summary,this analysis and testing method has high sensitivity,good precision and accuracy,low cost,simple operation,and wide applicability,making it easy for quality inspection institutions to refer to and apply.
作者
曹秀荣
路康
聂淼
徐盼
熊潇垚
CAO Xiurong;LU Kang;NIE Miao;XU Pan;XIONG Xiaoyao(Shangluo Agricultural Product Quality and Safety Center,Shangluo,Shaanxi 726000,China)
出处
《天津农业科学》
CAS
2023年第10期67-73,共7页
Tianjin Agricultural Sciences
基金
国家重点研发计划项目(2019YFC1606701)
陕西省农业科技示范推广项目(KJCX-2016-03)。
关键词
干木耳
有机氯及拟除虫菊酯类
农药残留
气相色谱测定
dried Auricularia
organic chlorine and pyrethroids
pesticide residues
gas chromatography determination
