Residue of spirotetramat, diafenthiuron and their metabolites in fruits and vegetables by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry
Received:October 28, 2018    Download the full
DOI：10.16801/j.issn.1008-7303.2019.0029
Key Words:QuEChERS  ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)  fruits and vegetables  spirotetramat  diafenthiuron  metabolites  residue
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Author NameAffiliationE-mail
LAN Feng Laboratory of Quality and Safety Risk Assessment for Fruit(Yantai), Ministry of Agriculture and Rural Affairs/Yantai Academy of Agricultural Sciences in Shandong Province, Yantai 265500, Shandong Province, China  
YAO Jie Laboratory of Quality and Safety Risk Assessment for Fruit(Yantai), Ministry of Agriculture and Rural Affairs/Yantai Academy of Agricultural Sciences in Shandong Province, Yantai 265500, Shandong Province, China  
ZHOU Xianxue Laboratory of Quality and Safety Risk Assessment for Fruit(Yantai), Ministry of Agriculture and Rural Affairs/Yantai Academy of Agricultural Sciences in Shandong Province, Yantai 265500, Shandong Province, China  
LIU Chuande Laboratory of Quality and Safety Risk Assessment for Fruit(Yantai), Ministry of Agriculture and Rural Affairs/Yantai Academy of Agricultural Sciences in Shandong Province, Yantai 265500, Shandong Province, China  
LI Xiaoliang Laboratory of Quality and Safety Risk Assessment for Fruit(Yantai), Ministry of Agriculture and Rural Affairs/Yantai Academy of Agricultural Sciences in Shandong Province, Yantai 265500, Shandong Province, China  
LU Zeqi Laboratory of Quality and Safety Risk Assessment for Fruit(Yantai), Ministry of Agriculture and Rural Affairs/Yantai Academy of Agricultural Sciences in Shandong Province, Yantai 265500, Shandong Province, China  
JIANG Wei Laboratory of Quality and Safety Risk Assessment for Fruit(Yantai), Ministry of Agriculture and Rural Affairs/Yantai Academy of Agricultural Sciences in Shandong Province, Yantai 265500, Shandong Province, China  
WANG Zhixin Laboratory of Quality and Safety Risk Assessment for Fruit(Yantai), Ministry of Agriculture and Rural Affairs/Yantai Academy of Agricultural Sciences in Shandong Province, Yantai 265500, Shandong Province, China 343684502@qq.com 
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Abstract:
      A method was developed for the quantitative determination of spirotetramat, diafenthiuron and their metabolite residues (spirotetramat-enol, spirotetramat-enol-glucoside, spirotetramat-mono-hydroxy, spriotetramat-keto-hydroxy, diafenthiuron-urea, diafenthiuron-amide) by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The samples were homogenized, extracted with V (acetonitrile):V(formic acid)=10:1, and cleaned-up by custom QuEChERS tubes. The separation was performed on a Shimadu Shim-pack XR-ODS column(75 mm×2.0 mm, 1.6 μm). The compounds were identified by MS/MS in positive electrospray ionization (ESI+) and multiple reaction monitoring (MRM) mode, and quantified by external standard method. The linearities of diafenthiuron-urea and diafenthiuron-amide ranged from 0.001 to 0.1 mg/L. And that of the other six compounds ranged from 0.005 to 0.5 mg/L, with the correlation coeffecients higher than 0.999 3. At the fortified level from 0.001 mg/kg to 0.5 mg/kg in pear, grape, watermelon, kale, celery and leek, the average recoveries of all the eight compounds ranged from 68% to 94% with the relative standard deviations varied from 5.4% to 15%. The limits of quantification (LOQ) of the analytes were 0.001-0.005 mg/kg. The method is simple, rapid, accurate and suitable for the confirmation and quantification of those eight compounds in fruits and vegetables.
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