摘要
目的建立一种利用液相色谱-串联质谱法同时测定茶叶中苯醚甲环唑、吡虫啉、噻虫嗪等24种农药残留的方法。方法称取2.00 g茶叶粉碎样经过8 ml超纯水浸泡30 min,用20 ml乙腈作为提取剂均质提取1 min,加盐离心3 min,取2 ml上层提取液过TPT柱净化,用10 ml乙腈.甲苯(2.3,体积比)淋洗剂淋洗,旋转蒸发浓缩至干,2 ml甲醇定容。用液相色谱-串联质谱法检测,基质标准曲线外标法定量。结果各种农药线性关系良好,相关系数均>0.99,定量限为2μg/kg~100μg/kg,24种农药的平均加标回收率在73.4%~99.4%,相对标准偏差在2.9%~9.3%。方法用于实际样品检测,检出进口红茶中噻虫嗪残留。结论该方法检测灵敏度高、准确性好,具有良好的回收率和稳定性。可满足茶叶中多种农药残留的日常检测需求。
Objective To establish a method for the simultaneous detection of 24 pesticide residues,such as difenoconazole,thiamethoxam,imidacloprid in tea by a liquid chromatography-tandem mass spectrometry method.Methods A total of 2.00 g grounded tea were soaked in 8 ml ultra-pure water for 30 min and homogenized with 20 ml acetonitrile for 1 min.The extracts were centrifuged with salt for 3 min.2 ml upper extraction solution was purified by TPT column,and eluted with 10 ml acetonitrile:toluene(2:3,V/V).The solutions were concentrated to dryness by rotary evaporation and concentrated in 2 ml methanol constant volume.The analytes were determined by liquid chromatography-tandem mass spectrometry and quantified by external standard method using matrix standard curves.Results The linear ranges of the method were suitable and the correlation coefficient(r)>0.99.The limits of quantitation were within 2μg/k-100μg/kg.The average recoveries of 24pesticide residues were 73.4%-99.4%,and the relative standard deviations were 2.9%-9.3%.The method was applied to the detection of pesticide residues in practical samples and thiamethoxam residues were detected in imported black tea.Conclusion The method is sensitive,accurate,rapid and reproducible,and can meet the requirement for the daily determinations of multi-pesticide residues in tea.
作者
徐文珍
陆思倩
吴娟
鲍维琪
姚芳懿
蒋沁婷
XU Wen-zhen;LU Si-qian;WU Juan;BAO Wei-qi;YAO Fang-yi;JIANG Qin-ting(Taizhou Municipal Center for Disease Control and Prevention,Taizhou,Zhejiang 318000,China;不详)
出处
《中国卫生检验杂志》
CAS
2022年第6期655-659,共5页
Chinese Journal of Health Laboratory Technology
基金
浙江省重点研发计划(2020C02024)。
关键词
茶叶
农药残留
液相色谱-串联质谱
Tea
Pesticide residues
Liquid chromatography-tandem mass spectrometry
