You Xiangwei, Sui Chengcheng, Li Yiqiang, Wang Xiuguo
Key Laboratory of Tobacco Pest Monitoring Controlling & Integrated Management, Tobacco Research Institute, Chinese Academy of Agricultural Sciences, Qingdao, Shandong Province, China.
J Sep Sci. 2017 Feb;40(3):702-708. doi: 10.1002/jssc.201601094. Epub 2016 Dec 22.
A rapid, reliable, and sensitive method is reported for the simultaneous analysis of pyrifluquinazon and its main metabolite NNI-0101-1H in fruits (strawberry and cherry) and vegetables (cucumber and tomato) using high-performance liquid chromatography coupled with tandem mass spectrometry. A modified, quick, easy, cheap, effective, rugged, and safe procedure was used for the sample pre-preparation. The target analytes were extracted with acetonitrile and then cleaned up using dispersive solid-phase extraction procedure with primary secondary amine. Sample analysis was performed using electrospray ionization in positive mode. Good linearities with the correlation coefficients higher than 0.9991 were obtained in the range of 1-1000 μg/L under the optimized conditions. The average recoveries of the pyrifluquinazon and NNI-0101-1H were in the range of 71.4-106.0% with the relative standard deviations 1.8-11.8% in all matrices at three spiked levels (10, 100, and 1000 μg/kg). The limit of quantification 10 μg/kg was set as the lowest spiked level. The developed method is reliable and effective for the routine monitoring of pyrifluquinazon and its metabolite NNI-0101-1H in fruits and vegetables to ensure food safety.
本文报道了一种快速、可靠且灵敏的方法，用于同时分析水果（草莓和樱桃）及蔬菜（黄瓜和番茄）中的吡蚜酮及其主要代谢物NNI - 0101 - 1H，该方法采用高效液相色谱 - 串联质谱联用技术。样品前处理采用改良的快速、简便、廉价、高效、耐用且安全的方法。目标分析物先用乙腈萃取，然后采用伯仲胺分散固相萃取法进行净化。样品分析采用正模式电喷雾电离。在优化条件下，1 - 1000μg/L范围内获得了相关系数高于0.9991的良好线性关系。在三个加标水平（10、100和1000μg/kg）下，所有基质中吡蚜酮和NNI - 0101 - 1H的平均回收率在71.4 - 106.0%之间，相对标准偏差为1.8 - 11.8%。定量限设定为最低加标水平10μg/kg。所建立的方法对于水果和蔬菜中吡蚜酮及其代谢物NNI - 0101 - 1H的常规监测以确保食品安全是可靠且有效的。
