摘要
制备了一种新型吸附材料铁磁性氟化石墨烯(FG@Fe 3O 4),用于萃取富集茶汤中10种含氟杀虫剂,结合气相色谱-串联质谱(GC-MS/MS)进行分析,研究含氟杀虫剂从茶叶到茶汤的浸出率。FG@Fe 3O 4同时具有石墨烯表面π电子和F原子,使FG@Fe 3O 4和含氟杀虫剂之间能够形成π-π共轭作用和F F相互作用而呈现出优异的吸附性能。通过扫描电镜、X-射线衍射、红外光谱以及振动样品磁力计对磁性吸附材料进行表征,并优化了萃取条件(吸附剂质量、洗脱溶剂种类和体积、萃取时间等),考察了不同材料的吸附效果以及自制FG@Fe 3O 4的重复使用次数。在优化的实验条件下,10种含氟杀虫剂在相应浓度范围内呈现良好的线性关系,相关系数R 2≥0.998,方法检出限为0.3~6.0μg/kg,3个添加水平的平均回收率在71.2%~108.4%之间,日内精密度RSD(n=6)在2.6%~8.7%之间,日间精密度RSD(n=5)在3.5%~7.8%之间。10份茶汤样品的检测结果显示,有2份样品中检出氟虫酰胺,2份样品检出氟虫脲,1份样品中检出氟硅唑,不同杀虫剂的浸出率不同。
A new magnetic sorbent named as ferromagnetic fluorinated graphene(FG@Fe 3O 4)was prepared for extraction and enrichment of 10 kinds of fluorine-containing pesticides in tea soups,which were then detected by gas chromatography tandem triple quadrupole mass spectrometer(GC-MS/MS).The transfer rate of fluorine-containing was also investigated.Due to theπelectrons and F atoms,FG@Fe 3O 4 could formπ-πconjugation and fluorous-fluorous interaction with fluorine-containing pesticides,and the magnetic sorbent displayed excellent adsorption performance for 10 kinds of fluorine-containing pesticides.Scanning electron microscopy,X-ray diffraction,Fourier transform infrared spectrometry and vibrating sample magnetometer were used to characterize the sorbents.The main parameters,such as sorbent amount,desorption solvent,extraction time were investigated.The adsorption properties of different sorbents and the recycle times of FG@Fe 3O 4 were also investigated.Under the optimum conditions,the linear relations were good in the corresponding concentration range with the correlation coefficients of more than 0.998.The method limits of detection(S/N=3)and method limits of quantitation(S/N=10)ranged from 0.3μg/kg to 6.0μg/kg and 1.0μg/kg to 20.0μg/kg,respectively.The average recoveries ranged from 71.2%to 108.4%and the intra-day precisions were 2.6%-8.7%at three standard spiked levels.This developed method was successfully applied for the detection of 10 tea soup samples,among which flubendiamide was detected in 2 samples,flufenoxuron was detected in 2 samples,and triflumizole was detected in one sample.The transfer rate of different fluorine-containing pesticide from teas to infusion was different.
作者
陈杰锋
梁明
冼燕萍
吴玉銮
温少楷
王斌
王莉
侯向昶
刘冬虹
CHEN Jie-Feng;LIANG Ming;XIAN Yan-Ping;WU Yu-Luan;WEN Shao-Kai;WANG Bin;WANG Li;HOU Xiang-Chang;LIU Dong-Hong(Guangzhou Quality Supervision and Testing Institute,Guangzhou City Research Center of Risk Dynamic Detection and Early Warning for Food Safety,Guangzhou City Key Laboratory of Detection Technology for Food Safety,Guangzhou 511447,China)
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2019年第8期1258-1266,共9页
Chinese Journal of Analytical Chemistry
基金
广东省质监局项目(No.2018PZ08)资助~~
关键词
铁磁性氟化石墨烯
含氟杀虫剂
茶汤
浸出率
气相色谱-串联质谱
Ferromagnetic fluorinated graphene
Fluorine-containing pesticides
Tea soups
Transfer rate
Gas chromatography-tandem triple quadrupole mass spectrometry
