摘要
建立了QuEChERS/气相色谱-三重四极杆质谱同时测定绿茶中35种农药残留的分析方法。样品经85℃热水冲泡,放凉后加入乙腈提取,采用200 mg N-丙基乙二胺(PSA)、200 mg十八烷基硅烷(C_(18))、50 mg石墨化炭黑(GCB)为分散固相萃取剂净化后,以Agilent HP-5MS毛细管柱(30 m×0.25 mm×0.25µm)分离,采用电子轰击离子源,以多反应监测模式测定,基质匹配标准曲线外标法定量。35种农药在10~1000µg/L质量浓度范围内线性关系良好,相关系数(r^(2))大于0.99,方法检出限和定量下限分别为1~5µg/kg和5~15µg/kg。在20、40、200µg/kg 3个加标水平下,绿茶基质中35种农药的平均回收率为70.3%~112%,相对标准偏差为1.6%~12%。应用该方法对30份市售绿茶样品进行检测,在4份样品中检出6种农药。该方法简单快速,灵敏度和准确度高,适用于绿茶样品中35种农药残留的日常检测。
A method of QuEChERS/gas chromatography-triple quadrupole mass spectrometry was es-tablished for the simultaneous determination of 35 pesticide residues in green tea.The samples were brewed with water at 85℃,then extracted with acetonitrile after cooling down.After purified with 200 mg PSA,200 mg C_(18) and 50 mg GCB,the analytes were separated on an Agilent HP-5MS capil-lary column(30 m×0.25 mm×0.25µm).The analysis was performed in electron impaction source under multi-reaction monitoring mode,and quantified by matrix-matched standard curve and exter-nal standard method.There were good linear relationships for 35 pesticides in concentration range of 10-1000µg/L,with their correlation coefficients(r^(2))larger than 0.99.The limits of detection and limits of quantitation were 1-5µg/kg and 5-15µg/kg,respectively.The average recoveries for 35 pesticides in green tea at the spiked levels of 20,40 and 200µg/kg ranged from 70.3%to 112%,with relative standard deviations of 1.6%-12%.30 commercially available green tea were detected by the proposed method,and 6 pesticides were found in 4 samples.The method is simple,rapid,sensitive,and accurate,and could be adapted for daily analysis and planed monitoring of 35 pesticide residues in green tea samples.
作者
高尧华
刘梦琳
李林杰
孙立
张晓文
阎炳
张鸿伟
GAO Yao-hua;LIU Meng-in;LI Lin-jie;SUN Li;ZHANG Xiao-wen;YAN Bing;ZHANG Hong-wei(Rizhao Customs,Rizhao 276826,China;Technology Center of Qingdao Customs District,Qingdao 266114,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2023年第10期1327-1334,共8页
Journal of Instrumental Analysis
基金
青岛海关“组阁揭榜”科研项目(QK202101)。
