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

引用本文: 宋伟, 周典兵, 郭春丽, 韩芳, 丁磊, 吕亚宁, 贾学颖, 郑平, 邓晓军. 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[J]. 分析化学, 2021, 49(9): 1587-1596. doi: 10.19756/j.issn.0253-3820.191683 shu

Citation: SONG Wei, ZHOU Dian-Bing, GUO Chun-Li, HAN Fang, DING Lei, LYU Ya-Ning, JIA Xue-Ying, ZHENG Ping, DENG Xiao-Jun. Determination of Multiresidue of Pesticide in Chrysanthemum by Magnetic Fullerene Dispersive Solid Phase Extraction with Liquid Chromatography-Tandem Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, 2021, 49(9): 1587-1596. doi: 10.19756/j.issn.0253-3820.191683 shu

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

宋伟 ^{1,2,
,} ,
周典兵 ^1,2, ,
郭春丽 ^1, ,
韩芳 ^1,2, ,
丁磊 ^1,2, ,
吕亚宁 ^1,2, ,
贾学颖 ^1, ,
郑平 ^1,2, ,
邓晓军 ^3,

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

通讯作者: 宋伟,E-mail:songwei1768@163.com

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

摘要: 合成了磁性富勒烯（Fe₃O₄@SiO₂@C₆₀），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，Fe₃O₄@SiO₂@C₆₀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 Fe₃O₄@SiO₂@C₆₀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Fe₃O₄@SiO₂@C₆₀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。

关键词:

English

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

1.
Technical Center for Hefei Customs, Hefei 230022, China;
2.
Anhui Province Key Laboratory of Analysis and Detection for Food Safety, Hefei 230022, China;
3.
Animal, Plant and Food Inspection & Quarantine Center, Shanghai Customs, Shanghai 200135, China

Corresponding author: SONG Wei, songwei1768@163.com

Received Date: 18 November 2019
Revised Date: 19 May 2021
Fund Project:
Supported by the Research Projects of the General Administration of Customs, China (No.2017IK108), the External Cooperation Program of Anhui Province, China (No.1804b06020349) and the Research Projects of Shanghai Science Committee, China (No.19395810100).

Abstract: Magnetic fullerene (Fe₃O₄@SiO₂@C₆₀) 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 Fe₃O₄@SiO₂@C₆₀ 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 Fe₃O₄@SiO₂@C₆₀ as adsorbent, extraction for 20 min under shaking, separation of the Fe₃O₄@SiO₂@C₆₀ by an external magnetic field, and elution two times with 1 mL of ethyl acetate. The result showed that Fe₃O₄@SiO₂@C₆₀ 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.

Key words:

Magnetic fullerene
/ Dispersive solid phase extraction
/ Liquid chromatography-tandem mass spectrometry
/ Pesticide residues
/ Chrysanthemum

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1.
沈阳化工大学材料科学与工程学院沈阳 110142

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

通讯作者: 宋伟,E-mail:songwei1768@163.com

English

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

Corresponding author: SONG Wei, songwei1768@163.com

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

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

通讯作者: 宋伟,E-mail:songwei1768@163.com

English

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

Corresponding author: SONG Wei, songwei1768@163.com

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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通讯作者: 陈斌, bchen63@163.com

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