磁性富勒烯分散固相萃取-液相色谱-串联质谱法测定菊花中农药残留  

Determination of Multiresidue of Pesticide in Chrysanthemum by Magnetic Fullerene Dispersive Solid Phase Extraction with Liquid Chromatography-Tandem Mass Spectrometry

作　　者：宋伟 周典兵 郭春丽 韩芳 丁磊 吕亚宁 贾学颖 郑平 邓晓军 SONG Wei;ZHOU Dian-Bing;GUO Chun-Li;HAN Fang;DING Lei;LYU Ya-Ning;JIA Xue-Ying;ZHENG Ping;DENG Xiao-Jun(Technical Center for Hefei Customs,Hefei 230022,China;Anhui Province Key Laboratory of Analysis and Detection for Food Safety,Hefei 230022,China;Animal,Plant and Food Inspection&Quarantine Center,Shanghai Customs,Shanghai 200135,China)

机构地区：[1]合肥海关技术中心,合肥230022 [2]食品安全分析与检测安徽省重点实验室,合肥230022 [3]上海海关动植物与食品检验检疫技术中心,上海200135

出　　处：《分析化学》2021年第9期1587-1596,共10页Chinese Journal of Analytical Chemistry

基　　金：海关总署科研项目(No.2017IK108);安徽省对外科技合作项目(No.1804b06020349);上海市科委项目(No.19395810100)资助。

摘　　要：合成了磁性富勒烯(Fe_(3)O_(4)@SiO_(2)@C_(60)),考察了其作为固相萃取吸附剂对菊花中农药的萃取富集性能,建立了超高效液相色谱-串联质谱(UHPLC-MS/MS)同时测定可食用菊花中9种农药(嘧菌环胺、苯酰菌胺、唑虫酰胺、嘧菌酯、吡唑醚菌酯、肟菌酯、唑螨酯、哒螨灵、辛硫磷)的分析方法。结果表明,Fe_(3)O_(4)@SiO_(2)@C_(60)对这9种农药有明显的吸附作用。考察了磁性分散固相萃取的影响因素,得到最佳的萃取和洗脱条件:以30.0 mg Fe_(3)O_(4)@SiO_(2)@C_(60)作为吸附剂,振荡萃取20 min,磁性分离,加1 mL乙酸乙酯洗脱液解析并重复2次。制备的Fe_(3)O_(4)@SiO_(2)@C_(60)材料具有良好的稳定性和可重复利用性。在0.005~0.1 mg/L范围内,9种目标农药呈现良好的线性关系,线性相关系数大于0.999。方法检出限在0.001~0.003 mg/kg之间,定量限在0.003~0.01 mg/kg之间。当添加水平为0.01、0.05和0.10 mg/kg时,回收率在71.0%~94.6%之间,相对标准偏差(n=6)在4.6%~11.3%之间。本方法操作简单、灵敏度高、分析速度快、成本低,适用于菊花中上述9种农药的定性与定量测定。Magnetic fullerene(Fe_(3)O_(4)@SiO_(2)@C_(60))was synthesized as a solid-phase extraction adsorbent for extraction and enrichment of pesticides in Chrysanthemum.Based on this,anultra-high performance liquid chromatography tandem mass spectrometry(UHPLC-MS/MS)method was developed for determination of nine kinds of pesticides,including cyprodinil,zoxamide,tolfenpyrad,azoxystrobin,pyraclostrobin,trifloxystrobin,fenpyroximate,pyridaben and phoxim in edible chrysanthemum.The results showed that the Fe_(3)O_(4)@SiO_(2)@C_(60)had obvious adsorption to cyprodinil,zoxamide,tolfenpyrad,azoxystrobin,pyraclostrobin,trifloxystrobin,fenpyroximate,pyridaben and phoxim.The influence factors of magnetic dispersion solid phase extraction were investigated,and it was found that a best extraction was obtained under the optimal conditions such as 30.0 mg of Fe_(3)O_(4)@SiO_(2)@C_(60)as adsorbent,extraction for 20 min under shaking,separation of the Fe_(3)O_(4)@SiO_(2)@C_(60)by an external magnetic field,and elution two times with 1 mL of ethyl acetate.The result showed that Fe_(3)O_(4)@SiO_(2)@C_(60)had good stability and reusability.All of the tested pesticides showed good linear relationship in the range of concentration 0.005-0.1 mg/L with correlation coefficients of greater than 0.999.The detection limits and the quantitation limits of nine target pesticides were in the range of 0.001-0.003 mg/kg and 0.003-0.01 mg/kg,respectively.When the addition levels of the pesticides were 0.01,0.05 and 0.10 mg/kg,the recoveries of the method ranged from 71.0%to 94.6%with the relative standard deviations(n=6)ranging from 4.6%to 11.3%.The method was simple,sensitive,fast and with low cost,and suitable for the accurate qualitative and quantitative determination of nine pesticides in chrysanthemum.

关 键 词：磁性富勒烯 分散固相萃取 液相色谱-串联质谱 农药残留 菊花 

分 类 号：O657.63[理学—分析化学] TS207.53[理学—化学]