超高效液相色谱-串联飞行时间质谱法测定绿茶中9种拟除虫菊酯类农药
超高效液相色谱-串联飞行时间质谱法测定绿茶中9种拟除虫菊酯类农药
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+加合离子, 苯醚氰菊酯、甲氰菊酯、氟胺氰菊酯易形成+加合离子。采用一级母离子定量, 9种拟除虫菊酯1~20 μg/L范围内线性关系良好(r2>0.99); 9种拟除虫菊酯的最低检出限均为1 μg/kg; 2~10 μg/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。
ObjectiveTo establish a method for the determination of pesticide residues of 9 pyrethrins in green tea. MethodsUltra high performance liquid chromatography electrospray ionization quadrupole-time-of-flight mass spectrometry was used for the quantification and fragmentation pathway of 9 pyrethroids. ResultsAfter extracting pyrethroids by QuEChERS method, the samples were easy to form + adduct ions under the positive ion mode, while + adduct ion were easy to form under the positive ion mode. The linear relationship of the method were significant within the range of 1~20 μg/L(r2>0.99). The limits of detection of all the 9 pyrethroids were 1 μg/kg. The recoveries within the range of 2~10 μg/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. ConclusionThe method is simple and efficient for the rapid screening of pyrethroid pesticide residues in green tea.
标题：超高效液相色谱-串联飞行时间质谱法测定绿茶中9种拟除虫菊酯类农药
英文标题：Determination of nine pyrethroids in green tea by ultra high performance liquid chromatogram tandem time of flight mass spectrometry
作者：
冯永巍 无锡市食品安全检验检测中心
许文艳 无锡市食品安全检验检测中心
郇宇 SCIEX中国应用中心
陆佩瑶 墨尔本大学
汪振炯 南京晓庄学院食品科学学院
中文关键词:拟除虫菊酯,超高效液相色谱串联飞行时间质谱,裂解规律,
英文关键词:pyrethroids,ultra high performance liquid chromatography tandem time-of-flight mass spectrometry,fragmentation pathway,
发表日期：2020-02-19
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