摘要
目的建立绿茶中9种拟除虫菊酯农药残留量检测的方法。方法采用超高效液相色谱电喷雾串联飞行质谱对9种拟除虫菊酯进行定量和裂解途径研究。结果样品经QuEChERS方法处理后上机,正离子模式下氟氯氰菊酯、氯氰菊酯、溴氰菊酯、氰戊菊酯、氟氰戊菊酯、四溴菊酯易形成[M+NH4]+加合离子,苯醚氰菊酯、甲氰菊酯、氟胺氰菊酯易形成[M+H]+加合离子。采用一级母离子定量,9种拟除虫菊酯1~20μg/L范围内线性关系良好(r^2>0.99);9种拟除虫菊酯的最低检出限均为1μg/kg;2~10μg/kg范围内回收率为85.2%~106.3%;相对标准偏差(RSD)≤6.1%。结论方法简便、高效适用于绿茶中拟除虫菊酯类农药残留的快速筛查。
Objective To establish a method for the determination of pesticide residues of 9 pyrethrins in green tea.Methods Ultra high performance liquid chromatography electrospray ionization quadrupole-time-of-flight mass spectrometry was used for the quantification and fragmentation pathway of 9 pyrethroids.Results After extracting pyrethroids by QuEChERS method,the samples were easy to form[M+NH4]+adduct ions under the positive ion mode,while[M+H]+adduct ion were easy to form under the positive ion mode.The linear relationship of the method were significant within the range of 1~20μg/L(r^2>0.99).The limits of detection of all the 9 pyrethroids were 1μg/kg.The recoveries within the range of 2~10μg/kg were 85.2~106.3%,and relative standard deviations(RSD)was no less than 6.1%.Quasi-molecular ions of 9 pyrethroids were fragmented from either ammonium adducts or hydrogenated molecules.Conclusion The method is simple and efficient for the rapid screening of pyrethroid pesticide residues in green tea.
作者
冯永巍
许文艳
郇宇
陆佩瑶
汪振炯
FENG Yong-Wei;XU Wen-Yan;HUAN Yu;LU Pei-Yao;WANG Zhen-Jiong(Wuxi Institute for Food Control,Wuxi 214142,China;Shanghai AB SCIEX Analytical Instrument Trading Co.Ltd,Shanghai,200335 China;University of Melbourne,Melbourne,3010,Australia;School of Food Science,Nanjing Xiaozhuang University,Nanjing 211171,China)
出处
《食品安全质量检测学报》
CAS
2020年第11期3516-3520,共5页
Journal of Food Safety and Quality
关键词
拟除虫菊酯
超高效液相色谱串联飞行时间质谱
裂解规律
pyrethroids
ultra high performance liquid chromatography tandem time-of-flight mass spectrometry
fragmentation pathway